trial exhibit 446

U.S. Department of Justice

Federal Bureau of Investigation

Washington, D. C

February

20s3 5-000 I

28, 2007

Norman GahnCalumet County District Attorney,s Office206 Court Street.Chilton, WI 53014

RE: State of Wisconsin v. Steven Averv

Dear Mr. Gahn:

I am wrJ-ting in response to a letter f rom rlerome F.Buting dated February 25, 2007, reguesting discovery in theabove-captioned matter. Eacrh request relating to the analysisperformed by the FBf Laboratory is addressed individually bel-ow.

1. "The protocol issu.e date is February 1_5, 2007...,

Enclosed is a copy of the relevant analysisprotocols utilized by the FBI Laboratory in this case.

2. "Any data on tests the FBI has done or cuIled... ',

There were no tests performed by the FBI thatdetermined the amounts of EDTA found in ordinaryhousehold or automotive objects.

3. "Any and all lab sheets, work sheets, bench sheets. .,,Enclosed is a copy of al-I of the fite material

generated by the FBI Laboratory relat,ing to theanalysis performed in this case. This materialincl-udes bench notes, computer printouts, chain ofcustody documents, and all other specific informationregarding the case. A CD Rom is also included withthis materiaL containing raw data files. These firescannot be accessed unless the proprietary softwarewhich is available from Thermo Finnigan, is installedon your computer.

{^r 4'l l-(i )

"*,a3{60TL

4.

5.

5.

.,

8.

"l\ny and all valiclation studies the FBI has done. .,,

Enclosed is a copy of the validation studies.

"Any and alL "limltation of detection" studies. . .,,

Information regarding studies referred to in theprotocol in this case is found in the material providedfor response 4.

"Any and aL1 "selectivity" st,udies referred to in...,,Information regarding studies referred t.o in t.he

prot.ocol in this case is found in the material providedfor response 4.

"Any and all "matrix effects" studies referred to...,,Information r:egarding studies referred to in the

protocol in this case is found in the material providedfor response 4.

"Citations to any and all "literatrlre" referred to. ."

Information r:egarding literature referred to inthe protocol j-n ttris case is found in the materialprovided for response 4.

"A list of any ancl all cases where Marc LeBeau. ."

Inasmuch as this request if not for documentationrelating to the pz:esent case or for documentationregarding underlyj"ng scientific data, it is beyond thescope of discovery.

"A complete curriculum vitae for any individual. . "

The analysis in this case was performed by UnitChief Marc A. LeBe:au. Chemist .fason Brewer was theTechnician. Examiner Madeline Montgomery was theTechnical Reviewer and Examiner Eileen Waninger was theAdministrative Rev'iewer in this case. A copy of theircurriculum vitae i.s enclosed.

"A1l data reflecti,ng the rate of degradation or..."fnasmuch as t.his reguest is not for documentation

relating to the present case, it is beyond the scope ofdj-scovery. This information can be researched by anydefense expert and is in the public domain.

t_0 .

1L.

2

€^t, +4 b

ro)

L4

1,2.

13.

15.

15.

L7.

18.

"Any complaints or negative performance evaluations. . .,,

Pursuant to IIBI Policy, a review of t,he Examiner,sfile for complainl-s or negative performance evaluationsmay be requested in writing by the prosecutor to t.heappropriate Chief Division Counsel, who will coordinatea search with appropri-aLe legal personnel atHeadquarLers. Laboratory personnel may not have accessto certain personnel files containing such information.

"Any and all insicle or outside prof iciency tests. . .',A copy of Lhe completed proficiency test summaries

for Unif Chief Marc A. LeBeau, Examiners EileenWaninger and Madeline Montgomery and Chemist ,JasonBrewer is enclosed.

"Laboratory chain of custody records, including a1I..."A11 informatlon, regarding chain of custody of

evidence for this case will be found in the case notesprovided for response 3.

"Copies of traceability documentation for sEandards. . . "

A11 informatjlon regarding traceability for thiscase will be founcl in the case notes provided forresponse 3.

"Instrument run 1og with identification of aII. . . "

A11 informati-on, regarding instrument run logs forthis case will be found in the case notes provided forresponse 3.

"Records of instrr.rment maintenance status and..."

Enclosed is er copy of the maintenance records oft,he j-nstruments used in the analysis of this case, fort.he time period surrounding the examination in thisarz c!a

"An error or contamination 1og covering any and a1l..."There were no instances of contamination in this

case. Had any instances occurred, the documentation,including actions taken, would be included in thematerial provided in response to request. 3. Anyrequest for documentat.j-on regarding error or

fa ++t'( 3)

contamination that occurred in other cases is bevondthe scope of the discovery.

1-9 . "Raw data f or the complete measurement sequence. . . ,,

A11 information regarding the raw data for thiscase, is found on the CD provided in response torequest, 3.

r hope this materi.al will assist vou in this effort.

,Joseph DiZinno, D.D.SAssistant DirectorLaboratorv Division

by

lfi /l'f t tL. ./ I/rr/ Robert TramSection ChiefScient.if ic Analysis Section

Enclosures

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NL:0r.l= 272.9273-5 F: - cESI SRM [email protected],272.50-273.501 MSSTAEILITYOS

.

ffilz. 248.+217 .5 Ft - cESI SRM ms2291.20@15,00 [246.50-247.50,272.50.273.501 MSSTABILITYOS

BTANK (neg blood, Dl H2O ext.)150

m/2.325.5-326.5 F: - cESI SRM [email protected] I299.50.300.50,325.50326.501 MSSTABILITYOS.

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Time (mh)

C :\Xcalibur\...\Stability\Stability09 5p

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C:D(calibur\...\Stability\Stabilityl 0 <up 02128tO7 06:13:31 BIANK (neg blood, Dl HZO ext.)

rrlz= 299.$300.5 F: - cESI SRM ms2

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C :U(calibu A...\Stability\Stabilityl 1 <<;Jlf 02128107 06:24:27 BLANK (neg blood, Dl H2O ext.)

NL: 0nlz= 272.1273.5 F: - cESI SRM [email protected] I246.50-247.*,272.5C273.501 MSSTABILTryI I

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nlz-282.&284.3Ft- cESI SRM [email protected]$2134.251 MSSTABILNYIl.

Timc (min)

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C:U(calibuA...\Stability\Stabilityl 2

1001

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mn= 282-8-2u.3 F: - cESI SRM [email protected]{1.r.251 MSsTAA[ttYt2

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NL: 0mlz= 272.5-213.6 Fi - cESI SRM [email protected]&247.50,272.50.273.501 MSsTA8tLtryl3

NL: 0r]/z= 24A.5-247.sFi. cESI SRM ms2291.20€115.0O I246.50,247.50,272.50-273.501 MSSTABILIryl3

C :\)(calibuA...\Stability\Stabilityl 3 02128107 06:46r08 BLANK (neg blood, Dl H2O ext.)

NL:3.80E3m/z= 299.$300.5 F: . cESI SRM rE2344.20@15,00 I299.5G300.50.325,50-326.501 MSSTABtltryl3-

'llma (mln) ,4q Tlne (min)

(,,\

C :U(calibur\...\Stability\Stabil ity 1 4 0212U07 06:57:01

NL:0ntz=272t.U?73.5F',. cESI SRMms229r.20@ rs.0o I246.50-247.50.272.sG273.501 MSSTABILITY,I4.

rnlz=282.9.2U.3F:- cESI Sru ms2303r0@'15.00 [282.7U28l ',t MSSTAB|L|Y14'

t{ qk/, t\

BLANK (neg blood, Dl H2O ext.).-f-i ^JryNL:0nt.|:= 299.5-300.5 F: . cESI SRM [email protected] I299.50-300.50.325.50326.sO1 MSSTABILITY1,I

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rVF 325.5326.5 F: - cESI SRM [email protected] I29S.5G300.50,325.5S326.501 MSSIABILTTY,I4-

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nm (nin) Tirne (rnh)

C:D(calibur\...\Stability\St bilityl 5

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0?i28107 07:07:51

NL:1.06E,1ntlz.216-5247.5F: - cESI SRM ms22s1.20O1s.00 I246.n-247.fi-272.5S,273.501 MSsTABtLtrYlS'

rlz= 282.9-284.3F: - cESI SRM ms2303.20Ots.@ [282.7$2r(.251 MSSTABILITYl5

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Card C extract (EDTA +)

100-l

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NL:4,61E4Nz=272.*273-5 F: - cESI SR[,] ms229r [email protected] {246.50-247.s0,272.50-273.501 MSSTAEILITYIs-

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mfu:325.5-326.5 F: - cESI SRM [email protected] [299.50.300.50.325.50.326.50t MSsTAErUTYls

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Tme (min)

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C:Xcalibur\...\Stability\Stabilityl 6 159 0?/28107 07:18:40 BLANK (neg blood, Dl H2O exl)

NL:0n!z'272.5-273.5F: - cESI sRM [email protected] [246,5e247.50,272.5G?73.501 MSSTABILITYI6.

rn/z= 245.$247.5 F: - cESISRM [email protected] [24650-?47.50,272.50-273.501 MSSTABIL|TYI6

m/z= 299.$300.5 F: - cESI SRM [email protected] l299.5&300.50.'325.50.326.50t MsSTAEILITY16'

Tim (min) Tim (mln)

C :U(calibur\...\Stability\Stabilityl 7 02128107 07:29:35

nlz- 246.5.247.5 F: - cESISRM [email protected] I216.5G217.fi.272.50-273.fit USSTABILITY,IT.

BLANK (neg blood, Dl H2O ext.)sP

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NL: otnlz= 272.5-273.5 Fi . cESI SRM [email protected] (216.fi-217.fi,272.50-273.sot MSsTABtLtrYlT'

Tinr (min) Tirr (min)

C:U(calibur\...\Slability\Stabiligl 8 fDP 0228107 07:40:31 Card D extract (EDTA +1

NL:1.14E5tnJl.272.9273.5 F:- cESI SRM [email protected],272.5G273.s01 MSSTABIL TY18

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r/2. 311.9,3'12.5 F: . cESI SRM [email protected] I311.5&312.501 MSSTABILITYIt

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rnlz= 282.8.2U.3F:. cESI SRM ms2303.20@ rs.00 t282.7$2114.25t MSSTA8ILITY18.

Tim€ (n{n) Tlme (min)

C :XcalibuA...\Stabil ity\Slability 1 I frp 0212W07 07151:26 BIANK (neg blood, Dl H2O ext.)

NL: O

ntlz= 272.1213.5 Fi - cESI SRM [email protected] I246.50-247.50,272.50-273.s01 MSSTABILITY,I9

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NL: O

tr/F 299.5.300.5 F: - cESI SRM [email protected] t299.50.300.50.'325.5e326.501 MSSTABILITYl9

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C :U(calibuA...\Stabil ity\Stability20 02128107 08:02:20

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BLANK (neg blood, Dl H2O ext.)

rvz= 325-$.326.5 F: - cESI SRM [email protected] {299.5&300.50,325.50.326,s01 MSSTABILTTY2O.

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rvz. 299.5.300.5 F: - cESISRM [email protected] MsSTABtLrry22'

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nn€ (rin) lim€ (min)

C:\j(calibur\...\Stability\Stabllity23

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nlz- 246.5.247 .5 F: - cESI SRM [email protected]{7.50.272.5e273.501 MSSTABtLnY23'

36

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Tlm (nin) Iim (rin)

C :l(calibur\...\Stability\Stab ilihr24 02f28107 08:45:49 Card F extract (EDTA +)

0'1 00-

80-

70-

55-

45-

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C:l(calibur1...\Stability\Stabilitv25 Tvg 02128107 Q8:56:43 BLANK (neg blood, Dl H2O ext.)

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n/z:325.$326.5 F: . cESI SRM ms23,t4,[email protected] [299.50.300.50.325.50.326.501 MSSTABILITY2S.

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Ttr. (rin)

C:XcalibuA...\Stabillty\Stability26 5-Df D2l2U07 09:07:38

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Tim (min)

rYz.3l't.$312.5 F: - cESISRM rc2356.00O15.00 [311.5e312.501 MSSTABILITY26

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Ikn€ (6in)

C:U(calibuA,..\Stability\Stability2T 02f28107 09:18:28

NL: 7.78E,1rnlz=272.5.273,5F: - cesl SRM ms22s1.20or 5.0o (

2,r6.5S247.50,272.50-?73.501 MSSTABILIW2T

NL: 6.33€3rr/F 246.5-247.5 F: . cESISRM ru229r.20O1s.m I246.55247.50.272.5G273.501 MSSTASILITY2T-

NL:1.55EFnlz.2V..8-N.3F: - cESI SR { ms230320@ r5.00 [282.7$284.25t MSSTABILITY2T.

Card G extract (EDTA +)5bg

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Tlmr (rnh)

C :U(calibuA...\Stability\Stability2S -1h? 02128107 09,29:23

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4,5283ttlz.248.*247.5 Fi - cESI SRil [email protected] [246.50-2,t7.50.2r2.so-2r3.soi MsSTA8[lIY2E

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Tlme (rnln)

C :U(calibur\...\Sta bility\S tability29 02/28107 09:40:17 BLANK (neg blood, Dl H2O ext.)

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\oI

nvz:325.5-326.5 F: . cESI SRM [email protected] [299.50.300.50,325.5S326.501 MSSTABILIry3o

f,r/u = 311.$312.5 F: . cESISRM [email protected] I311.5G312.501 MSSTABILITY3O'

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C:U(calibuA...\Stability\Stabilitv32'- Tb{ 0?i28,C/ 10:12:51 BLANK (neg blood, Dl H2O ext.)

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dtlzE 216.5247.5 F: . cESI SRM trt32291.20@r5.@ I246.50-247.50,272.5G273.501 MSSTABILI']Y32

2.138Ailz= 282.U28/..3F:. cESI SRM ns23O3.20O15.@ [282.75.2t14.25t MSSTABILTTY32

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C:Xcalibu 4...\Stability\Stability33 0428107 10:23:40

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tlF 282.&2U.3 Fi - cESI SRM [email protected] [282.7$21425t MSSTASILNY$.

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rTri:= 325.5-326.5 F: - cESI SRM [email protected] |299.50-300.50.32s.so-326.50i MssTABtLtTY33'

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C:u(catibuA,,.\Stability\Sjqj!!ty35 aiF 0?i28107 10:45:25 BTANK (neg blood, Dl HzO ext.)

nlz=272.5-273.5 Fi. cESI SRM ms2291.20Or5.001246.50-247.50.272.5S273.501 MSSTABILIry35.

r!z=216.5-247.sFi- cESI SRM [email protected] [216.*247.fi.272.sS273.501 MSSTABILITrcS'

rfilz= 292.t12E4.3 F: - cESI SRM [email protected]&..7r2U.25t MSSTABILIT}'35

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Tim lmin)

lxt: u.utj . 19.u2 5M: 3(iNL:1.94E3 |

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C :U(calibur\...\Stability\Stability36 0212407 10:56:17 Card J extract (EDTA +;

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-lnlz- 272.$27!.5 F: - cESI SRM ms2291.20Or5.00 [246.50-247.50.272-50.273.501 MSSTABILI1Y36.

rvz= 325.5.326.5 F: - cESI SRM [email protected] MSSTABILITY36.

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C :[(calibuA...\Stability\Slability3T A2l2U07 11:07:10 BIANK (neg blood, Dl H2O exl.)

NL:0trlz- 272.$273.5 F: - cESI SRM [email protected] MSSTAAILITY3T

flVz=299.$300.5 F: - cESI SRM [email protected],325.50-326.501 MSsTABtLnr3T

-

Tm(min)

n/z' 31 1.5-312.5 F: - cESI SRt4 ms23s5.00o1s.00 [311.50-312.501 MSSTAEILITY3T

a(-y ++('

C:U(calibur\...\Stabilih^Stabilitv3E -jlF 0?/2U07 11:18:05

t*rrule0-l

NL: 2.16E3rtlz?272.12?3.5F: -cESI SRM ms2291.20@15,00 [246.50-247.50.2t2.50.273.501 MSSTAB|UW3S'

Ilr. (min) J.'.oa'lltu)


NL:1.55E3r/z= 299.$300.5 F: - cESI SRM [email protected] [email protected] MSsTAEtLrTWs'

REg!t€.l.EoE

Tim (ndn)

C :U(calibur\...\Stability\Stability39 100 ppm EDTA

,*-lru-l

s0l

tolru-l

,o-j

85-]

ro-]

rrlro-]

*'l*-l

nrulmin)

rv.= 325.5-326.5 F: - cESI SRM ms234,[email protected]&300.50.325.s0.326.s0t MSSTABILITY3g.

I'lz-2a2.8.2U,3Ft. cESI SFIM tr8230320@1!;.001282.7$28.1.2q MSSTABILITY39

f:,K{r

0?/2U07 1 1:39:48

NL; 0nlzr 2f2.s273.5 F; - cESI SRM ms229120O15.001248.*21f .9,272.5G273,501 MSSTABILITY4O

BLANK (neS blood, Dl H2O ext.)

Tlm(mir)

C :l(calibuA...\Stab ility\Stability4 1 TbF 0228[07.11:50:40 BLANK (neg blood, Dl H2O ext,)

RI:0.00-10.02 SM:3GNL: O

o?

io

io

tilz=272.*273.5Fi - cESISRM [email protected] [24650.247.50,272.50273.501 MSSTABILITY4I

tr'lz=246.6247.5F: - cESI SRM rns229r 20O'r 5.00 I246.50247.50.272.50273.501 MSSTABILITY4l

rr'z= 2a2.&-2E/.3 F: - cESI SRM rns230320@t s.00 [282.75-2eQ51 MSsTABtLrn'41

{*

lr<r: u.oo - ru.uz sM: rG

NLOrn/z= 299.t300.5 F: . cESI SRM rsz

l#:"38J3.S,t325.50-326.50t MSSTABTLITY4'I

-

:2.06E3nvz:325.$326.5 F: - cESI SRM ms2

li3:338J333t32s.5G326.501 MSSTABILITY4T

L4 to

,- C :U(calituril..\EDTA\Brewer\O22807U2801 0A28107 03:31:28 EDTA neg blood/H2O extract To{

ds

:r2

6

NL: O

nlF n2,*7135Fi- cESI SRM nE2291.20@,|5.00 [246.9.241.fi.272.50.273.501 MS22001

R

i!c{3.t.9

E

NL:2.55E3rn/z:290.$300.5 F: - cESI SRM [email protected] MS22fJJ1

nft= 311.$312.5 F: -

ESISRM G2356.00O1s.00 [3r 1.5G312.sO1 MS22Eo1

nJZ.216.*217,5Fi - cESISRM ffi229r20Ct15.0O I246.5G247.50.272.5O-Zr3.5Ol MS2?@1

Ifm ln{n) Tlm(rnn)

Cr +q

rofnl*-1

*-l

C :l(caliDuA...\EDTA\BreweA022807tE,2B02

8oo

tuu

0A28107 03:42i41'--ir D

100 ppm EDTA J'f

nJz= 24Ei.5.217.sFi - cESI SRM ms2291,[email protected] [246.5(F217,50.272.5G273.so1 MS22802

NL: 1.56E4m/r:299.$300.5 F: . cESI SRM [email protected] I299.50.300.50.325.50-326.sot MS22802

m/:= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MS22802

m/2.311.$312.5Fi-cESI SRM [email protected] I311,5O.312.501 MS22eo2

R

6E

eo..:o

Tim(mh)

Sample Name:

Comment:

Seq u e n ce---E DTA-sta bi I ity-n eg ion . sld [O pen]

BI-ANK (neg blood, Dl l't9o ef.)n

Study:

Client

Laboratory:

Company:

Phone:

C : Xcal i bu Amethod s\EDTA_Neg_

Sample Name:

Comment Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path Inst Method

Unknown STABILITYO2 02 C :\Xcalibu tlData\E DTA\Brewer\Stability u:\ GilrDunmemoos\Eu I A_Neg_swaDs

Proc Method CalFile Position njVol Level Sample Wt Sample Vol ISTD Amt

1 5.0 0.000 0.000 1.000

ozl..xl'tSF

Seq uence--E DTA-sta b i I ity-neg i on. s I d [Open]

Sample Name:

Comment

card extract

Study:

Client

Laboratory:

Company:

Phone:

Sarnple Type ile Name Sample lD Path lnst Method

Unknown STABILIryO3 01 :\Xcalibu nData\EDTA\Brewenstablllty C: U(calibur\methods\EDTA-Neg-Swabs

Proc Method CalFile Position lnjVol Level Sample Wt Sample Vol ISTD Amt

2 5.0 0.000 0.000 1.000

Sample N (neg blood, Dl H2O ext,

Comment: Study:

Client

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path lnst Method

Unkno,vn STABILITYM 01 C:Xcalibu AData\EDTA\BreweAStability C :Xcali bu r\methods\E DTA_Neg_Swabs

Proc Method CalFile Position lnjVol Level Sample Wt Sample Vol ISTD Amt

1 5.0 0.000 0.000 1.000

otlt-rl"t@

Sample Name:

Comment:

(neg blood, Dl H2O ext.

Study:

Client

Laboratory:

Company:

Phone:

Proc Memoo CalFile Position njVol Level Sample Wt Sample Vol ISTD Amt

1 5.0 t.000 0.000 1.000

ffifrffiisffittrffiat€t*fttffifftffffitffittffiffiatlffilillta*tttttt#ittltt*tffifftttill*iit*txlfft'ttttft

Sample Name:I

comrnent studY:

Client:

Laboratory:

Company:

Phone:

Seq u en ce-- E DTA-sta bi I ity-ne g ion. sl d [O pen ]

f; {r/ e,( q+\

page 3 /

lDil Factor I

n006---l

rttatt*tt**frtt**tt**hitttttittt*iaftittit*t*t**Ht#fr tat*frit*tF6l*ttrt*HttttftffaitlttattHat*ttttffti*trattrtifffft*ta*tt

otftl"t'ft?


Unknown STABILIWOs 01 C fXca[i ou rtOata\EDTA\Brewer\Stability C :Xcali bu r\m ethods\EDTA-Neg-Swa bs


Unknown STABILITYO6 01 C :\)(calibu r\Data\E DTA\Brewer\Stabili$ :v(calibur\metnocls\ts IJ I A_Neg_swaDs

Seq uence---E DTA_sta bi I ity_neg i o n. s ld [O pen]

Sample t,tame:tl

Study:

Client:

l-aboratory:

Company:

Phone:


Unknown STABILIryOT 01 g: u(caltbunDaE\ts D I A\Hre\r/er\Stabrlrty u:xcallbunmemods\tsD I A_Neg-liwabs

Proc Method CalFile Position InjVol Level Sample Wt SampleVol ISTD Amt

5.0 0.000 0.000 1.000

Sample Name:

Comment: Study:

tllient:

l-aboratory:

Oompany:

Phone:

sample lype File Name Sample lD Path lnst Method

Unknown STABILITYOS 01 C:XcaliburlData\EDTA\BreweAStability : \Xcalib u r\m ethods\EDTA_N eg_Swabs

Proc Method CalFile Position lnjVol Level Samole Wt Sample Vol STD Amt

5,0 3.000 0.000 1.000

[* +na( +s1

page4'

ovl*1"1{!P

Sample Name:

Comment:

Seq u e n ce---E DTA_sta bi I itlneg i on . sld [O pen ]

Study:

Client:

Laboratory:

Company:

Phone:

+)


Unknown STABILIWOg 01 C :\)(calibuAData\EDTA\BreweAStabili$ C :U(cal i bu r\m ethods\E DTA-Neg_Swabs

Proc Metnod CalFile Position njVol Level Sample Wt Sample Vol ISTD Amt

4 5.0 0.000 0.000 1.000

Sample Name:

Comment: Study:

Client:

Laboratory:

Company:

Phone:

,neg


Unknown STAEILITYlO 01 c: \xcali bu RDaIa\EDTA\B rewer\Stability C :\Xcalabu r\methods\E DTA_N eg_Swabs

fr r'(L,( qL,\

page 5

ouluel"l.S.roF

Seq u e n ce--E DTA_sta b i I ity_n eg ion . s I d [O pe n ]

Sample Name:

Comment:

ext.

Study:

Client:

Laboratory:

Company:

Phone:


Unknown STAEILITY1l 01 :U(cal i bu AData\EDTA\Brewer\Stab ility C:XcdibuAmethods\EDTA_Neg-Swabs

Proc Method Cal File Position InjVol Level Sample Wt Sample Vol ISTD Amt

5,0 0.000 0.000 1.000

Sample Name: lIJComment Study:

Client:

Laboratory:

Company:

Phone:


Unknown STABILITY12 01 u:\ cattDunuata\Eu I A\tsrewen$EDilrty C:\Xcalibur\methods\EDTA_Neg_Swabs

ttaaittttt*ff tttittttit*t*

fl,t+a(v t)

page 6 '

or- f urJ"'l'{nP

Sample Name:

Comment:

Seq uen ce---E DTA-sta bi I ity-neg i on . sld [O pe n]

BI-ANK (neg blood, Dl H2O eX.

Study:

Client:

Laboratory:

Company:

Phone:

Proc Method CalFile Position InjVol Level Sample Wt Sample vol ISTD Amt

1 5.0 0.000 0.000 1.000

Sample 11366'

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path lnst Memod

Unknown STAEILITYl4 01 C :Xcalibu r\Data\EDTA\BreweAStabili$ :Xcalibu Amethods\E DTA_N e g_Swabs

Proc Method CalFile Position Injvol Level Sample Wt Sample Vol ISTD Amt

1 5.0 0.000 0.000 1.000

5. qu"( as)

pageT'

orlrsl-t'gP

S eq u ence--- E DTA-stab i I ity-neg i o n. sld [O pen]

Sample Name:

Comment StudY:

Client:

Laboratory:

Company;

Phone:


Unknown STABILITY1S 01 C:U(cali bu r\Data\EDTA\8 rewe r\Stabi lity :Xcalibur\methods\E DTA_Neg_Swa bs

Proc Method CalFile Position InjVol Level Sample Wt Sample Vol ISTD Amt

o 5.0 0.000 0.000 1.000

Sample Name:

Comment:

(neg ext.

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name SamDle lD Path lnst Method

Unknown STABILITYl6 01 c: u(caltDu r\Data\Eu I A\tsrewensEDrlrty :\Xcalibur\methods\EDTA_Neg-Swabs


1 5.U 0.000 0.000 1.000

orl*1.1,s,P[*'/'/-,

( +q\page 8/

Seq u e n ce-- E DTA-sta b i I ity-neg io n. s I d [O pen]

Sample Name:

Comment:

neg blood, Dl H2O ext.)

Study:

Client:

Laboratory:

Company:

Phone:

trffiffiffiffiffif,*tftl*'t*llffftltf.ttttffi**tttlllttttttt.ttffltffitftsfrttlllltaftt*tt.tta

Sample Name: Card D extract (EDTA +

Comment: Study:

Client:

Laboratory:

Company:

Phone:


Unknown STABILITYlT 01 C:\)(calibuAData\EDTA\BreweAStabil ity : Xcalibur\methods\EDTA-N eg-Swabs

Proc Method CalFile Position InjVol Level Sample Wt Sample Vol ISTD AMt

1 5.0 0.000 0.000 1.000

o.lrrl't'av?5z,tu+

/5o)page 9'

S eq u ence--- E DTA-sta bi I ity-n eg i o n. sld [O pe n ]

Sample Name:

Comment:

(neg blood, Dl H2O ext.)

Study:

Client:

Laboratory:

Company:

Phone:

Itiff rtrttff tffi ffi F.tttff tlttl*llt#tltttrtff ttft$tff lllff lfr tltAttltff I

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:

Sample Type Fild Name Sample lD Inst Methotl

Unknown STABILITY19 01 C:Xcali bur\Datra\EDTA\Brewer\Stability :Xcdibu Amehods\E DTA-N eg-Swabs

Proc Method CalFile Position lnjVol Level Sample Wt Samole Vol ISTD Amt

1 5.0 0.000 0.000 1.000

foquo( s,)

page'10

ovlt'||t"1'$'P

EDTA Stability Study:

Ten EDTA-preserved blood spot cards were analyzed following approximately 33months of storage at room temperature. The free acid form of EDTA was detected in alll0 of the spot cards. The EDTA-iron complex was detectable in 6 of the l0 spot cards.Failure to identify the EDTA-iron complex was based on the lack of the less abundantproduct ion (m/z 326). The more abundant m/z 300 for EDTA-iron was present in all l0ofthe spot cards.

5o +v6G4

CASE FILE

t, q+b(')

7;l-M*a'ct.t6)

ffiffi'@ 2501 Investigation Parkway

Quantico, Virginia 221 35

REPORT OF EXAMINATION

To: Milwaukee Date: Febru ary 26,2007Squad 6/GBRASA Gerald E. Mullen Case IDNo.: 62D-MW-443$*bl

Lab No.: 070201013 PM GH

Reference : Communication dated January 3 0, 2007

Your No.:

Title: STEVEN AVERY;TERESA HALBACH-VICTIM (DECEASED)DOMESTIC COOPERATION-HOMICIDE

Date specimens received: February 1,2007 arrd February 6,2007

The following items were examined in the Chemistry Unit:

Q46 Swab (Item 9569)


Q48 Swab (ltem9572)

Q49 Liquid blood sample from STIIVEN AVERY (Item 9803)

K2 Two control swabs (Item 9802)



This report contains the results of the chernistry examinations.

Page 1 of3

For Official Use Onlv

14t6( s+\

Results of Examinations:

Specimens Q46-Q49 and K2-K4 were analyzed for the presence of ethylenediamine-tetraacetic acid @DTA).

Specimen Q49 was listed as a liquid blood sample from STEVEN AVERy in a l0milliliter (mL) lavender-top blood tube. It contained approximately 5.5 mL of blood. EDTA wasidentified in specimen Q49.

Specimens Q46-Q48 were reported to be collection swabs of blood stains from thecrime scene associated with the death of TERESA HALBACH. Specimens K2-K4 were reportedto be control swabs collected in relation to the Q46-Q48 swabs. BO1R, either as the free acid oras the EDTA-iron complex, was not identified on the e46-e4g or K2-K4 swabs.

The analysis for EDTA was carried out using liquid cluomatography/tandem massspectrometry in both positive and negative electrospray ionization modes.

Remarks:

EDTA is an anti-coagulant and en4rme inhibitor that is commonly used in bloodcollection tubes. Blood specimen collectiorr tubes containing EDTA have lavender-colored topsand are the most common collection tube used to collect reference specimens for DNA testing.

The concentration of EDTA in its free acid form in a drawn blood tube is typically1000-2000 milligrams per liter (mg/L), depending on the volume of blood and the.up*ity oith.tube. At this concentration, the free acid and salt forms of EDTA are soluble in blood. EDTAreadily forms water-soluble chelates with nearly all heavy metals, including iron in blood.Aqueous extractions of dried bloodstains allLow for the isolation of EDTA (both as the free acidand as the EDTA-iron complex) if present.

Using the procedure employed irr this case, EDTA is readily identified at aconcenfration of 13 mglL. Additionally, ELITA is also detectable when a 1-microliter drop ofEDTA-preserved blood is analyzed

For questions about the content of this report, please contact Unit Chief Marc LeBeauat (703) 632-7408.

Page2 of3

07020t013 PM GH


€o ++e,

1st)

For questions about the status of remaining forensic examinations, if applicable,please contact Request coordinator Michael vanArsd-ale at (703) 632-gg09.

The submitted evidence was returned under separate cover of communication.

Marc A. LeBeau, PhDChemistry Unit(703) 632-7408

Technically reviewed and any identifications and associations confirmed bv:

This report contains the opinions/interpretations of the examiner(s) who issued the report.

Page 3 of3

070201013 PM GH


&.++,-/5r\

7-251 (7-13-e8)

The Enclosed material for

LABORATORY DIVISIONSUPPORTING DOCUMENTATION ENVELOPE

Case ID/ Sub LzD-,/uW - qV ?1,3

IA Serial #

Please Print Clearly

LtT3e*n supports LaboratorY RePort

Ilor

Name

LabNumber(s) 11 O-z'o | 013Or WO Number

Case ID, Sub and Serial

Chain of Custody

Communication and ActivitY Log

Notes

Instrument Prrnt Outs, Charts, Graphs

Negatives

Photographs

ECS Search Slip

Shipping Invoice

DescriptionofEnclosures itl -

\ )'rv'n Nole g - J'.f Jv<

7s .- l2 Pr+r-gS

P hsh' ,{ {po't- {izes ' I /''f"EF ssL b,J,^- * b I Pn r,rs

please Return This Ilnvelope And All contents To The

a

7-.lJBEr'io 0-06)

r^rl ni.-^u---.-,Y,-Lg.

Hrui FBI Laboratory

MilwaukeeSquad 6/GBRASA Gerald E. Mullen

Reference:

Your No.:

Title:

K2

K3

K4

This report contains the results of the chemistry examinations.

Page 1 of3

2501 Investigation Parkway

Quantico, Virginia 221 35

REPORT OF EXAMINATION

Date: February 26,2007

Case ID No.: 62D-MW'443$-(ol

Lab No.: 070201013 PM GH

STEVEN AVERY;TERESA HALBACH-VICTM (DECEASED)

DOMESTIC COOPERATION -HOMICIDE

Date specimens received: February 1,2007 and February 6,2007

The following items were examined in the Chemistry Unit:




Q49 Liquid blood sample from STEVEN AVERY (Item 9803)

Communication dated January 30, 2007

Two control swabs (Item 9802)

Two control swabs Qtem 9801)

Two control swabs (Item 9800)

For Offrcial Use Only

6o ++t( ss)

Results of Examinations:

specimens Q46-Q49 and K2-K4 were analyzed for the presence of ethylenediamine-tetraacetic acid @DTA).

specimen Q49 was listed as a liquid blood sample from sTEVEN AvERy in a 10milliliter (mL) lavender-top blood tube. It contained uppro*i*utely 5.5 mL of blood. EDTA wasidentified in specimen e49.

Specimens Q46-Q4s were reported to be collection swabs of blood stains from thecrime scene associated with the death of TERESA IIALBACH. Specimen, rz-r+ were reportedto be control swabs collected in relation tg s. Q46-Q4g .wabs. EDTA, either as the free acid oras the EDTA-iron cornplex, was not identified * trr. q+o_e4g or K2-K4 swabs.

The analysis for EDTA was.carri.ed out using liquid chromatography/tandem massspectromety in both positive and negative elechosprayfonization modes.

Remarks:

EDTA is an,anti-coagulant and enzyme inhibitor that is commonly used in bloodcollection tubes' Blood specimen collection tubes containing EDTA have lavender-colored topsand are the most common collection tube used to collect refeience specimens for DNA testing.

The concentration of EDTA in its free acid fonn in a drawn blood tube is typically1000-2000 milligrams per liter (mg/L), depending on the uolu*, of blood and the capacity of thetube' At this concentation, the free acid and saliforms of EDTA are soluble in blood. EDTAreadily forms water-soluble chelates with nearly alldt;etals, including iron in blood.Aqueous extactions of dried bloodstains allowfor the isolation of EDTA (both as the free acidand as the EDTA-iron complex) ifpresent.

Using the procedurl.e.mnlg-red in this case, EDTA is readily identified at aconcenbation of 13 mglL. Additionally, EDTA is also detectable when a l-microliter drop ofEDTA-preserved blood is analyzed. 4 r-'uvr'

For questions about the content of this report, please contact unit chief Marc LeBeauat (703) 632-7408.

Page 2 of 3

070201013 PM GH

For Official Use Only

f, ++t"( s'i)

/

For questions about the status of remaining forensic examinations, if applicable,please contact Request coordinator Michael vanarsiare -i''

rloz>632-gg09.

The submitted evidence was returned under separate cover of communication.

Marc A. LeBeau, phDChemisty Unit(703) 632-7408

Technically reviewed and any identifications and associations confirmed by:

Date:

This report contains the opinions/interpretations of the examiner(s) who issued the report.Page 3 of3

070201013 PM GH


fn vqb(cr,\

7-25{ (7-13-98)

The Enclosed material for

LABORATORY DIVISIONSUPPORTING DOCUMENTATION ENVELOPE

Case ID/ Sub (,zD-/uW-aV?A3lA Serial #

orlPlease Print Clearly

Lr&et'u supports Laboratory RePort

Description of Enclosures

\ )rnqin'de .- l7

't Na

P l,,ul.' o{ {po'l- 9i zccl

. tli7_. frhl/

d!- k0 Panu

Case ID, Sub and Serial

Chain of Custody

Communication and ActivitY Log

Notes

Instrument Print Outs, Charts, Graphs

Negatives

Photographs

ECS Search Slip

Shipping Invoice

Name

LabNumber(s) 01 tSt'o I 0 13Or WO Number

F ssL b,d"- - 6l Pnrcs

Please Return This Envelope And All Contents To The

(Rcv. 0l-3 l'2003)

FEDERAL BUREAU oF tI{rtEsTlGATlOIU

Fron: MilwaukeeSquad 6/GBRA r ,^^^\Coatact,:SAGeraldE'MuIlen,(920)432-3868

APProved B-yr Greco RaYmond A

Drafted By: Mullen Gerald E:d1g 070201013

Cage ID #: 62D-MW-44363 (Pending)-5b

Tit,Ie: STEVEN AVERY iTERESA I{ALBACH-VICTIM (DECEASED)

DOMESTIC COOPERATION-HOMI CIDE

Slraopeie:Summaryo{captioned'matterwithrequestforaPProPriate examination'

PackageCoPy:Beingforwardedunderseparatecoveraretrhefollowing iEemst To 3e Srlr.#q#

1) one box conta'ining vial human blood'- it,'1'c^rDt? -

fut,,':J'oFg- tro(oziulto

2) envelopes containing swabs from crime scene

DetaiLs: Teresa Halbach was reported missing by family members

"" ii7o3 /2oot. sn. was rasr seln on 10/3r/2005 on the propertyof steven Avery "n" "t""

a salvagg yard with his family' Halbach

wa' Eaking pirotogiipit" of a vehiEle that was for sale as she

worked for the Auto'Trader: magazine' Numerous search warrantswere executed on the Averlr property and. significant evidence was

,""o.r"r"d implic"iing Steireir Alrery_1n the murder of TeresaHalbach. The Cal;;;i --*tty Sfreriff , 'Jerry Pagel' has requested

the assistance of the FBI fbr laboratory examinations.

Precedeace: DEAD]TINE B I 09 / 2007

To s Laborat,ory

DaEe: orl3 o/2007

Attn: Scientific Analysis SectionChemistry UnitMark Lebeau

stevenAverlgwasreleasedfromprisonin2003afterbeing exonerated for I rape conviction by DNA evidence' A vialof Avery,s Uf ooe, which wls drawn and, ueld to exonerate him inthe rape conviction, was maintained at the Manitowoc County Clerkof Courts Office. Avery's defense has aLleged the-investigatorsfrom the Manitowoc county sheriff's Department used this vial of

blood to plant evidence lrc the crime scene implicating Avery inmurder of teresa Halbach. This vial of blood contains EDTA'

RE;rURI.{ E\TIDENCP

ro lGirv nu Ys;-DIvIsloNa-,/ q4b

/t.'>\ "l4tltu/

To: Laboratory From: MilwaukeeRe: 62D-MW-44363 , 0L/30/ZOOI

The purpose of this reguest is to estabrish thepresence of EDTA, in the vial of -blood, thereby eliminating theallegation that this vial was used. t,o plant evidence.

Averyrs trial is scheduled !o began on o2/os/zool.special Prosecut,or calumet county District Attorney'Ken Kratz,has -requested rhis examinaEion bi complered by oilbg/io07 ro beused ag rebuttal evidence.

2

C-^/ (Vr-fuz)

4/,w"l-,"1'=

cf)

-c)NOf.-

To:Re:

I-,,aboratory From: Milwaukee62D-MW-44363, Ot/30/2007

LEAD (g) I

Set Lead, 1: (Action)

I,ABORATORY

AT OUANTICO, VA

Chemstry Unit conduct appropriate examination of vialof blood to determine the presence of EDTA. Conduct relevantcomparisons to swabs from crime scene. Conduct degradationanaiydis of blood. Tt is requested t,his examination be-ompieted by 03/Og/2007. The point, of contact from the WisconsinOepirt,ment ;f .Tustice is Assistant Attorney General Norm Gahn at(920) 418-4087.

ti

RETURN] EVIDENCETO MIL\TAUIiLE DiVISIO}tr

fy 44r-

I

(Y)

Oc)NONO

( r+)/VJ/1.,. Ln

7-243 (Rev.3-3r-04) FBI Laboratory

Chain-of-Custody Los G@'FYd'.- :, ..'e/ (-.-r'-,f

I Laboratory No.: O7O2O1Or a 'ffin* Case II) No.: G z\ - 1tr 14 - 11StoS

Tracking No(e).: 7 11O Ll b7 9 '/1/1 |

Opened for Retrieval of Communication ny: I//

Date: 2/ / /07

-

tr Shipping Container Damage

ECC Comments:

Container(s) Received Via Date Contributor

I ?nVfecl Ex -b- /-n-drtb,,.D tf ifoz FBf 7,t ilua"-Lcc

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Container(s) Delivered Date Remarla

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(quLaboratorv Number:

070201013 I

tui\ A, {Chain-of-Custodv Paoi t/ of '

@cv.3-31-04) FBI Laboratory

Chain-of-Custody Log

-aboratory No.: O?O&OIO lg Case ID No.: l9 t"8- fnUJ -4 4AUs

TrackingNo(s).: Tlqo 4rc73,:ii1q I

Opened for Retrieval of Communication Uy Or*, A l L0l2&Z

tr Shipping Container Damage

Container(s) Received Via Date Contributor

t Bu,vfutex -/(rnufur{L,r 4ol^-, fil iluJ0ruko& . ul

faLrc,u_

ECC Comments:

s) Delivered B Date Remarks

I bati *lomiad,,tML)' Into ECU Storage zl rll?&z

-) E&r w{efrirentor BSafe oshelf

I uryFrom ECU Storage r1lffi 2.1I4o 0{qJ

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Items Received:

a19,fj.U ,Hlr,,nn (h&ffi:"R- *l+/or

a ',\WQNIa49. ff|,,,,ffi*a, 4#ryt a2-@7

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Chain-of-Custody Page _ of '

7-243a (Rev. 3-3 I -04)

FBI Laboratory

Chain-of-Custody Log

uao'atorvNo.: fr7o2@1a73 caserDNo.: 6zD- Mw- ug6ltr, Request Coordinato/s Logd Innaunit Logtr Other

Unit Name:

Unit Name:

Unit Name:

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Delivered B fpd Date Remarksa46-a48;NEz.NE4.

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7-245 (Rcv. 6-l 9-00)

FBI LaboratoryActivity and Communication Log

Laboratory No.: 0nOA,Ol O t e, Case ID No.:

Activity/Communication and OutcomeDate

L/J/-qBy: CO.(.

D-Mw -*Vib.

pzl--, t*__By: .'*

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By:

(z\ 4lWrl ,nln[^r'/+A

Violation{s):rstic Police Cooperation

Violation date:Violation Location:

Victim:HALBACH, TERESA

Cross Reference:

Remarks:

Lab No: 070201013 PM GH

City: Milwaukee, WisconsinAgency: FBI

Form: Electronic Communication, 01/30/2007CaselD: 62D-MW44363 Seriat:Latent Number:Contributor No: 62D-MW-44363

Subiect:AVERY, STEVEN

30

ECC Delivered to Unit:

Previous Submission(s)

o6t2270L2 PM PvMilwaukee, WisconsinFtsIElectlonic CoE'!. : t2/19 /2006Qs:15-tl5 Ks : NE IteE!:

^-r 11{005 PM PV NNlraukee, Wisconsin

-4ectronic Coua. : Ll/ 01 / 2006Qs:13-1tl

06u08009 PM PvMilwaukee, WisconsinEBIElectronic Co&a.. : tl/02/2006Qs:11-12

060118254 QcMilwaukee, Wisconsin

Electronic Conln. : Ol/ 04/2006 ELna]-:04/ LL/2OO6Qs:3-10 NE Jtahe:l

051123009 PM MRl'lilwaukee, WisconainEBTElectlonic Co@,. : tl/L6/2005Qs:1-2

el Method and No: Federal Express .7190 4673 4441xes - l Date Received: 0210112007 -More

Received in ECC: 0?0il20070210712007 12:03:28 PM . mvanarsdale fo 4+,

( tr)/vw'

?-lzbln

ECU- I (Rev.7f27D005)

Evidence Control UnitEvidence Check-In Notes

Laboratory Number: 070201013 PM Case ID: 62D-MW_44363

Received via FedEx one sealed box, tracking number 7lg0 4673 444l,containing:one sealed box containing:six sealed paper bags:

bag labeled "9569" contained:one sealed envelope containing:

Q46 Swab (Item 9569)bag labeled " 957 4' contained:one sealed envelope containing:

Q47 Swab (ltem 9574)bag labeled "9572" contained:

one sealed envelope containing:

Q48 Swab (ltem9572)bag labeled "9801" contained:one unsealed envelope containing: *envelope sealed in ECU*one unsealed box containing: *box sealed in ECU*NE2 Two control swabs (ltem 9801)bag labeled "9802" contained:one unsealed envelope containing: *envelope sealed in ECU*one unsealed box containing: +box seak:d in ECU*NE3 Two control swabs (Item 9802)bag labeled "9800" contained:one unsealed envelope containing: *envelope sealed in ECU*one unsealed box containing: *box sealed in ECU*NE4 Two control swabs (Item 9800)

+q-bZ-r)

a /vw-l- ,1^u

ECU - I (Rev.7/27D005)

Evidence Control UnitEvidence Check-ln Notes

Laboratory Number: 070201013 PM Case ID: 62D-MW-44363

* indicates unopened in ECU to preserve examinations, descriptions taken from packaginglEC

Received one sealed FedEx box TRK# 7190 4673 5091 (discarded in ECU) containing one sealedbox containing one sealed container containing one closed vial containing one purple top tube of liquidblood:

Q49 Liquid blood sample from STEVEN AVERY (Item 9g03)

Initials of Preparer,&Date: 717 l0+ uPaee 1of-p

fu+ut-(tt)

L.- Ln4fi,\,-l . , [,'rl

7-2 (Rev. 7-10-06)

Federal Bureau of InvestigationLaboratory Division

LABORATORY WORK SHEET

To: Milwaukee Date: February 1,2007Squad 6/GBRASA Gerald E. Mullen case rD No.: 62D-Mw-44363

LabNo.: 070201013 PM

Reference: Communication dated January 30, 2007

YourNo.:

ritle: STEVEN AVERY;TERESA HALBACH-VICTIM PECEASED)DOMESTIC COOPERATION.HOMICIDE

Date specimens received: February t,2007

Specimens:



Q48 Swab Stem9572)

K: -NEZ-'[' Two control swabs (Item 98,01)

.<'n

K2_ $83-'l' Two control swabs (Item 9802)

Kq NB+IF Two control swabs (Item 9800)

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Check-In Date:CHEaIsT:' BKEATCA

case ID *: (Ll - nil ,- ll16 s E:raminer: Le B.+q

Mode .Reccived: '/E USPS tr FedEx d DelivcredBY:

E CT)

Tracking #:

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d Boxes (# I ) tr PaPer Bags (# )

tr Plastic Bags (# ) tr EnveloPes (# )

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Condition of Extemal Container(s):,

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GENERAL DESCRIPTION OF' EVtr)ENCE AIT{D COIT{TAINER,S:

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Initials: JFS

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GENERAL DESCRIPTION OF EVIDENCE AND CONTAINERS (continued):

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Initials: X6$Lab* aloLul cttz

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a'{L f,'(tu 15 e 1ztUF t;-1fc>4 {lv48 ,',/ Dtr.t< pp-utNtS\ S.T.+^l

ft-ry1 bfrJ4ea1,zD NEtL l6Nt-fronl Siu tTt:i/

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Mode.Receive& )/E USPS tr FedEx u/ Delivued By

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e/noxes (# | ) tr Paper Bags (# )

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tr Cans (#

tr Othec

Condition of External' Container(s):

{*optr Seal(s)llabel(s) tr Othen (Co,r,"',eot Below)

GENERAL DESCRIPTION OF' E\TIDENCE A}ID CONTAE{ERS:

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5taqedcg ('rror'to/3-- n"J, ,1/ ') r,vtr]a6 fF*ttr€T,I

5/ +'lb('?")

o, l!6 lz---1

0211512007

Blood spot sizes (l uL, 5 uL, 10 uL)

OJoloto\sTpP

{v ++t-('it)

\t',/

?;t,hre ESr ,M/o/e

TANDEM MASS SPECTRAPOS ESI MODE

Pos GontrolB

Pos GontrolA

Q49 LOD - lul

Pos GontrolA

Q49 LOD - 2uL

responseion ratiopass / fail



100.0PASS

Diagnostic lons (m/z)160 m/z 132 24791367.6 13928 7492.5100.0 15.2 8.2

67724.8 9790.4 6929.4100.0 14.5 10.2PASS PASS PASS

Diagnostic lons (m/z)160 m/z 132 24791367.6 13928 7492.5100.0 15.2 8.24349.5 0 1803.5100.0 0.0 41.5PASS FAIL FAIL

Diagnostic lons (m/z)150 m/z 132 24791367.6 13928 7492.5100.0 15.2 8.2

1807.7 698.718.3 7.1

PASS PASS

/,f

/-lt.J'

2yha

ey lqb1q^\

fta4ar"rnls -

ur@

zlrt,lot07b7atol3

lW

C:\Xcalibuirdata\Brewer\070201 013\21 623

RT:0.89S#:66M:837425

SilA 70AA:77063

NL:1.25E5fit/z= 159.S160.5F: + c ESI Full [email protected] Ms21623

10(

9{

9(

T5

70

ffilz= 246.5-247 .5F: + c ESI Full [email protected] I125.00-315.001 MSzlozJ

@oo

o

=ao

: 2.08E5Tlc Ms21623

+ c ESI Full ms2 [email protected] I

02116107 M:Q2:32 Pos. Cont. A (MAL EDTA ext.)

21623#60-70 Rr: 0.81-0.95 Av: 11F: + c ESI FuLI ros2 293.00015.00 f 1r<

r32 .07122 ntI ?? qa

f J6.9b160.04160.80

t7 4 .64

zzz.6z247 .L4249.00293.24

Intensity Relative280.5 0.31

I3928.0 15.24

549.3 0.71244.9 0.21

91367.5 100. 000.1 0.00

253.4 0.28955.5 1.05'709.4 0.?8r92.3 0 .27

7 492.5 I .20985.0 1. 08

3323. ? 3. 54

{,v +Vt/ at\

"t,lzt,lo:- a'-

0l ozol o l3

C:U(catibur\'data\Brewer\07020 1 O1 3U1 626

100-t

"u_1

RT:0.92S#:68AA:535858

NL: 9.69E4n/z= '1 59.5-1 60.5F: + c ESI Full [email protected] t1 25.00-31 5.00t'MSztoz6

S#:64AA:51139

RT: 0.65S#:4EAA:,28/'O

NL:2.18E5Tlc Ms 21626

OZ16107 04:35:06

+ c ESt Fuil ms2 [email protected] I 1

Pos. Cont. B (Q49 ext.)

21625#63-7I RT: 0. B5-0.9G Av:9F: + c ESJ Full rns2 [email protected] I r25 . ..

12' n 1

l qa "oL60 .02

?)7 Cn

230.95)'1A a)246.93z03.y5214 .80275.48)oa )e

Intensity Relative' 9790.4 14.46

986.1 1.46413.8 0.61442.9 0. 65

57724.8 I00 . oo0.4 0.00

965.3 1.431a?1 1 1 11

1213.l. 1. ?96929.4 la.2327!.3 0.40

1631.9 2.4L499.9 0. ?{

2089.4 3.09

zl'o[ot[* ++u

/o)

C:t(calibur\data\Brewer\070201 O1 3\2 1 629

RT:0.89S#:65AA: 19603

NL:4.34E3trYz= 159.5-,160.5F:+c551PrU."t

?!3:3381333r"'21629

. I tlE2S#: &lM:2958'10(

9:

9C

80

75

70

c

o

o

NL:2.10E5Trc Ms 21629

0?/16107 05:07:38 Spot LOD, 1uL e49

.ii-sii,rrmsi'ziiioit6rf ,ioirii;ioo'jislSq1Oo_ 160

2152e#54_6s @P:. + 6 951 Fult rns2 [email protected] t t2Sn/z Intensity Relative

159.95 4349. q r no ^^?19'?s i;,ii:; ';;:;;

293.33 3758.0 85.40

& qq-Lz't<\

lltlvu [01

o

6

+cESl

C:Xcalibur\data\BreweA070201 01 3U 1 632

RT:0.9'lS#:67AA: 39228

02116107 05:40:13

ms2 [email protected] 1 tZS.oo-Sts.oO1

Spot LOD,2 uL Q49

L632#65-6't Rr: 0. 88-0.91 tt-F: + c ESI FulI ns2 293.00G15.00 Im/ z Intensity Relative

L25 . ..NL:9.04E3n/z= 159.5-160.5F: + c ESI Fult ms2

?!3:33.9133&r"'21632

L32 .64

160.01fo/.uu200.30z90.Jb250.08?q? 11

1807.7 18.323227 .3 32.119865.0 100.00758.7 1.69

1044.3 10. 59598.? 7.08

2064.3 20.935131.0 52. 15

S#:47AA:5E91

1 00-l

ru-J

ro-]

ru]

'ltuJ

'l65-l-l @

6

o.=

,ArrQ?

$\lfl /\t\P,

NL:1.68E5Ttc Ms 21632

€s vub -ulr,"lol/ ,:,\

Instrument Method: EDTA pos Swabs.meth

LCQ Instrument Method

Creator: AdministratorLast. modifiedt 2/!6/07 by Administrator

MS Run Time (min) : 10. 00

Divert, Valve: Dot used durinq run

MS Detector Settinqs:

Segment l- fnformation

Duration (min) : 10. O0Number of Scan Events: l_

Tune Method: EDTA_Pos_CfD

Scan Event Details:1: Pos - (293.0)->o(L2!;.0-315.0)

MS/MS: CE 15. O? ttsow 1.0

t, 44bz; z\

Page L of 2

QlaYcr a | 3Or/rc lLco'J

Friday, February 16, 2OO7 05:07203

Inst.rument, Method: EDTA Pos Swabs . meth

Waters 2690 LC Svstem

Injector parameters:Syringe draw rate (pI/sec):2.50Injection vol-ume (p1) :5

Pump settings:Solvent A:5:95 ACN:Water + 0.06t NH4OHSolvent B:BSolvent C:CSolvent D: DMin pressure (PSI):0Max pressure (PSI) :5000frha rl- nrr{- nrl{- . Dr*-. - -essureCha rf nrrf nrrf . Nnry1g]

Gradient program:Time(min) Flow(m]/min) A(E) B(t) C(S) D(t) Curve0.00 0.30 100.0 0.0 0.0 0.0 Llnear - G

3 .00 0. 30 100. 0 0. 0 0.0 0. 0 Li_near - G

Timed events:Initial states:

Switch L:No change. Switch 2:No change '

Switch 3:No changeSwitch 4:No chanqe

firne (min) Event Action Parameter0.00 Switchl No chanqe

Friday, February 15, 2007 C)5 : 07 ; 03 /^

'-v q'/ b

,/; \

Page 2 of 2

c'1aL,r I cl3crrfrr"ltc-'1

Sample Name:

C.,mment:

(neg Dl H2O ext.)

Seq uenc e---07 0201 0 1 3_Pos. sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path Inst MethodUnknown 21601 C : Xcali bur\Data\B rewer\07 0201 0 1 3 U:\ calrbur\methods\EDTA Pos Swabs

Proc Method Cal File Position InjVol Level Sample Wt lSample Vol ISTD Amt

1 5.0 0.000 0.000 0.000

Sample Name:

Comment:

Neg. Control(-EDTA blood swab ext.)

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path Inst MethodunKnown 21602 02 C: U(calibu r\Data\Brewer\07 020 1 01 3 C:Xcalibur\methods\EDTA pos-Swabs

Proc Cal File Position InjVol Level Sample Wt Sample Vol ISTD Amt2 5.0 0.000 0.000 0.000

f* v+,-/cq\

/1/wo7ola I o l3

czf rr lz-o1-l-tP

page 1

Sample Name:

C^-rment:

Sequenc e---070201 01 3_Pos. sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path Inst MethodUnknown 21603 01 C:Xcal ibu r\Data\Brewer\07 020 1 0 1 3 C:Xcalibur\methods\EDTA pos Swabs

Proc Method CalFile Position njVol Level Sample Wt Sample Vol ISTD Amt1 5.0 0.000 0.000 0.000

t***t************************************t

Sample Name:_r-lComment Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path lnst MethodUNKNOWN 21604 01 C:U(calibur\Data\BreweA07020 1 0 t3 C:Xcalibur\methods\EDTA pos SteG

Proc Method CalFile Position InjVol Level Sample Wt Sample Vol STD AmtI 5.0 0.000 0.u00 0.000

t********************** **t*******t***t******************************+i******a*****

t" q(u( r"")

oaoe2

a1c'tat ol3orf rt,f Lool

-ir$

Seq uenc e--07 020 1 0 1 3-Pos. sld [Open]

Sample Name:

C^rment:

extract

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Samole lD Path lnst Method

Unknown 21605 03 C:\)(calibur\Data\Brewer\070201 0 1 3 C:Xcalibur\methods\EDTA Pos-Swabs

Proc Method iCal File Position InjVol Level Sample Wt Sample Vol ISTD Amt

3 5.0 0.000 0.000 0.000

Sample Name:IBLANK (neg blood, Dl H2O ext.)

Comment:

****************t***************t***t***i*********t*****

Study:

Client:

l-aboratory:

r0ompany:

Phone:

AA/.,p/"c1o'Lc'lol3o.tlrUltu,'1

JDRr{+ qvL,(/or)

oaoe 3

Sample Type ile Name Samole lD Path lnst Method

Unknown 21606 01 C tXcatiOu rtData\Brewer\07020 1 0 1 3 C:U(cal i bu r\methods\E DTA-Pos-Swabs


1 5.0 0.000 0.000 ]o.ooo

Sequence--07 0201 0 1 3_Pos. sld [Open]

Sample Name:

C^"nment:


t***t****s*tt********t*i**i***********************tft

Study:

Client:

Laboratory:

Company:

Phone:

Study:

Client:

Laboratory:

llompany:

Phone:

Sample Name:

Comment:

extract


Unknown 21607 01 C :\XcalibuAData\B rewer\07 0201 0 1 3 C:U(calibur\methods\EDTA Pos Swabs


1 5.0 0.000 0.000 0.000


unKnown 21 608 04 C: \Xcal ibu i\Data\Brewer\07 0201 0 1 3 C:Xcalibur\methods\EDTA Pos Swabs

Proc Method lCalFile lPositionInjVol Level Sample Wt Sample Vol ISTD Amt

145.0 0.000 0.000 0.000

t*****************************************f****************************t*i*******t************************************t

fu q(b(t,r)

nanc 4

01o'La 1 o l3ozlrt,iu.,,7

Tttl

Sample Name:

C - -ment:

Sequence---07 020 1 0 1 3_Pos.sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21609 01 :XcalibuAData\Brewer\07020 1 0 1 3 C:U(calibur\methods\EDTA Pos Swabs


1 5.0 U.OOU 0.000 0.000

Sample Name:

Comment:

neg blood, Dl H2O ext.)

Sample Type File Name Sample lD Path nst Method

Unknown 21610 01 C : \Xca I ibu AData\Brewer\07 0201 0 1 3 C:U(calibur\methods\EDTA Pos Swabs

Proc Method Cal File Posrtron InjVol Level Sample Wt Sample Vol ISTD Amt

1 5.0 0.000 0.000 0.000

*****tt********************t***t

{* qt/L,,( t ol;

nane 5

ol a'Lo\ o13

c'lf tt l)-"--7-rbF

Sample Name:

C- -ment:

Sequence---07 020 1 01 3_Pos.sld [Open]

K3 extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21611 05 C:Xcalibu r\Data\Brewer\070201 0 1 3 G:\XcaltDur\memo0s\tsu I A Pos Swabs


5 5.0 0,000 U.UUU U.UUU

**tt*********t*************

Sample Name: BLANK (neg blood, Dl H2O ext.

Comment: Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21612 UI C:U(calibu r\Data\BreweA070201 0 1 3 C:Xcalibur\methods\EDTA Pos Swabs


1 5.0 0.000 0.000 0.000

**i**********************

4/1/t'/olo2-olol3

c,'r- [ tt, I L.t c,lI_oF

5r,V4r-( r"v)

nenc A

Sample Name:

(^ .ment:

Sequenc e---07 0201 01 3_Pos.sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21613 01 C :XcalibuAData\Brewer\O70201 0 1 3 C:XcalibuAmethods\EDTA Pos Swabs


1 5.0 0.000 0.000 0.000

*i******************t********************************t**ist**************t*t*t*t***ti**1************#**f,**t****t**

Sample Name:

Comment:

Q47 extract

Study:

Client:

Laboratory:

Company:

Phone:

21614 C : Xcal i bu AData\B rewer\O7 0201 0 1

Proc Method Cal File Position lnjVol Level Sample Wt Sample Vol

o 5.0 0.000 0.000 0.000

*********************

{* vvt( rcs)

clola't t'r13

a'>ltt-lro"J.r1rP

Seq uen c e---07 0201 0 1 3_Pos. sld [Open]

Sample Name:

C- -ment:


Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21615 01 C:Xcalibur\Data\Brewer\070201 0 1 3 C:U(callbur\methods\EDTA Pos Swabs

Proc Method CalFile Position InjVol Level sample wt Sample Vol ISTD Amt

1 5.0 0.000 0.000 0.000

Sample Name:

Comment Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21616 01 C : \Xcalibu r\Data\B rewer\07 0201 0 1 3 C:U(calibur\methods\EDTA Pos Swabs

Proc Method tCal FileI

Position njVol Level Sample Wt rSample Vol IST

1 5.0 0.000 0.000 0.000

t*********t****************************************************t***********l***********************l

fx a4r-lrou\

naoe I /

O-7c>Lt t cl3olf ru lz'"1

Tbp

Sample Name:

/^- -'rment:

Seq uenc e---07 0201 0 1 3_Pos. sld [O pen]

K4 extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21617 07 C:U(cal ibur\Data\Brewer\07020 1 0 1 3 C:U(calibuAmethods\EDTA Pos Sw,bs

Proc Method Cal File Position lnjVol Level Samole Wt Sample Vol ISTD Amt7 5.0 0.000 rJ.000 0.000

*t*******i*****************r******

Sample Name: (neg blood, Dl H2O ext.

Comment: Study:

,Client:

Laboratory:

Company:

Phone:


Unknown 21618 01 C :\Xca libu r\Data\Brewer\07 0201 0 1 3 C:U(calibur\methods\EDTA Pos Swabs

Proc Method Cal File Position lnjVol Level Sample Wt Sample Vol iISTD Amt

1 5.0 0.000 0.00u 0.000

*****************************

5, qvL.

"!::')

0lcLolol3oLl lt I z-"c 1

wF

Sample Name:

C^-ment:

Sequenc e---07 020 1 0 1 3_Pos. sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21619 01 C:U(calibur\Data\Brewer\070201 0 1 3 C:U(calibur\methods\EDTA Pos Swabs


1 5.0 0.000 0.000 0.000

Sample Name:

Comment:

extract

Study:

Client:

Laboratory:

Company:

Phone:

sample lype File Name Sample lD Path Inst Method

Unknown 21620 08 C:U(calibur\Data\Brewer\07020 1 0 1 3 C:Xcalibur\methods\EDTA Pos Swabs

Proc Method Cal File Position InjVol Level lSample Wt Sample Vol STD Amt

I 5.0 0.000 0.000 10.000

******************t**************t

/o q+GoJoLo\ o\3

6Ll \b I t-,'1-TI'F

( t,s1nana 1O

Sample Name:

C^-rnent:

Sequenc e---07 020 1 0 1 3_Pos. sld [Open]

BLANK (neg blood, Dl H2O ext.

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Samole lD Path Inst Method

Unknown 21621 01 C:\)(calibur\Data\Brewer\070201 0 1 3 C:D(calibuAmethods\EDTA Pos Swabs


1 5.0 U.UUU 0.000 U.UUU

*************

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:


unKnown 21622 01 C:\)(calibur\Data\Brewer\07020 1 0't 3 C:XcalibuAmethods\EDTA Pos Swabs

Proc Metnod Cal File Position InjVol evel lSample WtI

Samole Vol Amt

1 5.0 U.UUU 0.000 0.000

f************

/* ,/'/ ('(t"o)

oaoe 1 1

ol0Lol O l3oLlit l2oc-i

T0fl

Sequenc e--070201 01 3_Pos. sld [OpenJ

Sample Name:I

O^-rnent: Study:

Client:

Laboratory:

Company:

Phone:

******t*********i*t*****t*****************************t*****t*****************

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:

******************

F*********t*******************ft ************************************

{* L/4 6( tro)

naoe 12

o-l 0LOl0l3ui-ltClzooT

i-uP

Sample Type File Name Sample lD Path lnst MethodUnknown 21623 09 : \Xcallbur\Data\Brewer\07020 1 0 1 l : U(ca libur\methods\E DTA_poLSwaG

Proc Method Cal File Position InjVol Level Sample Wt Sample Vol ISTD Amtv 5.0 0.000 0.000 0.000

ype File Name Sample lD Path Inst Method

Unknown 21624 01 C: \Xcalibur\Data\Brewer\O7 0201 01 3 C : U(cal i bur\meth ods\E DTA_pos_Swa bs

Proc Method Cal File Position InjVol Level Sample Wt Sample Vol ISTD Amti1 5.0 0.000 0.000 0.000

Sequence--07020 1 0 1 3_pos.sld [Open]

Sample tlame: ]C^*rment Study:

Client:

Laboratory:

Company:

Phone:

**************************l**t********************************f******ft*i*******************t*************t*****************************i*******

Sample Name:

Comment:

Cont. B (Q49 ext.)

Study:

Client:

Laboratory:

Company:

Phone:

***tt********i************t**********i*********************************************

Sample Type File Name Darnpte tu lHam Inst MethodUnknown 21625 01 :Xcalibur\Data\Brewer\0i0201 0 1 l \ACat tDu r\method s\EDTA_Pos_swa bs

Sample Type File Name Samole lD Path lnstUnknown 21626 10 C:DGalibur\Data\Brewe^0

Method Cal File Position InjVol Levet ]Sampte Wt lsampteTol Amt10 5.0 u.000 0.000 0.000

f* 44a(r"\

nana 4 2

ol oLcl a l70Lll6l t-oa1

-r1rg

Sample Name:

C^rment:

Sequence---07 020 1 0 1 3_Pos. sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21627 01 u: \xcattbur\Data\Brewen070201 0 1 : C : Xca I i bu r\m ethod s\EDTA_Pos_ Swabs

Proc Method Cal Fite Position lnjVol Level Sample Wt Sample Vol ISTD Amt

1 5.0 0.000 0.000 0.000

**************************s*****t*

Sample Name:

Comment:


Study:

Client:

l-aboratory:

Company:

Phone:

************t******************


Unknown 21628 01 C :\Xcal ibu r\Data\Brewer\07 020 1 0 1 3 U:V\calrDur\methods\EDTA Pos Swabs

Proc Method Cal File Position InjVol Level Sample Wt Samole Vol ISTD Amt

i1 5.0 0.000 0.000 0.000

{* ,L{a(r t ,a)

oaoe 14

ol o Zo\0lloLllvl i,oc)

aoP

Sample Name:

C^'nment:

Sequenc e---07 020 1 0 1 3_pos.std [Open]

{u avu,( tra)

oaoe 15

LOD, 1uL

Study:

Client:

Laboratory:

Company:

Phone:

*************l*t*********t****t*******************************************t*tt**tf***********t********************t***********r****************

Sample Narne:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:

*************************'*************************************************************************t********************

o1s7.o I c 1jc:>ltulz,"

7

IV,F

Sample Type File Name Sample lD Path Inst MethodUnknown 21629 11 C:Xcalibur\Data\Brewer\07020 1 0 1 3 u : v(cattb u r\methods\EDTA_pos_Swa bs

Proc Method CalFile iPositio- InjVol Level Sample Wt Sample Vol ISTD Amt1 b.0 u.0u0 0.000 0.000

Sample Type File Name Samole lD Path nst MethodUnknown 21 630 01 C:\)(calibuirData\Brewer\070201 01 l C:\)(calibur\methodstEDTA pos Swabs

Proc Method CalFile Position njVol Level Sample Wt ]Sampte Vol ISTD Amt

i50 0.000 0.000 0.

Sample t{ame:l'lu^Tment: Study:

Client:

Laboratory:

Company:

Phone:

Sample Name:

Comment:

Spot LOD,

Study:

Client:

Laboratory:

Company:

Phone:

Seq uenc e---07 0201 0 1 3_pos. std [OpenJ

{* uu,(r,v\

naoe 16

***************t************************************t**t**t**t********ti*******************

r**************t***************************************

/l,/r,U61aL.. I allcz{rr"f Laol

avP

Sample Type Frle Name Sample lD Path Inst MethodUnknown 21631 01 C:U(calibuAData\BreweJ\o2020 1 O 1 l :U(calibu r\methods\EDTA_poi Swabs

Proc Method CalFile Position InjVol Level Sample Wt lSampte VolI

ISTD Amt1 5.0 0.000 0.000 0.000

Proc Method Cal File Position InjVol Level Sample Wt Sample Vol ISTD Amt12 5.0 0.000 0.000 0.000

Sample Name:

C^-ment:

BLANK (neg I H2O ext.)

Sequence---070201 01 3_Pos.sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name lSamole lDI

Path Inst MethodUnknown 21633 01 :Xcal i bu r\Data\Brewer\07020 1 0 1 :l G:u(calibur\methods\EDTA pos Swabs

Proc Method CalFile Position InjVol Level Sample Wt Sample Vol ISTD Amt1 5.0 0.000 0.000 0.000

*****t*****t****t***************i********t*

f'u +rle'(its)

oaoe 17

oloLol o13

ctzlrt lLo"-lavF

Vial List---C. Xca li bu r\methods\brewer\07020 1 0 1 3\070 20 1 0 1 3 Pos. sld

Position Sample Type Level Sample lD Sample Name

3

Unknown 1 BLANK (neg blood, Dl H2O ext.)

Unknown 02 Neg. Control (-EDTA blood swab ext.)

Unknown 03 K2 extract

4 Unknown 04 Q46 extract

c Unknown 05 K3 extract

o Unknown 06 Q47 extract

7 Unknown 07 K4 extract

I Unknown 08 Q48 extract

I Unknown 09 Pos. Cont. A (MAL EDTA ext.)

10 Unknown 10 Pos. Cont. B (Qa9 ext.)

11 Unknown 11 Spot LOD, 1uL Q49

12 Unknown 12 Spot LOD, 2 uL Q49

{o ++l-(r,)

nana 1

QloLol al3

" tlrc I loo.tT\tP

a

TANDEM MASS SPECTRANEG ESI MODE

Pos ControlA

Q49 LOD - 1uL

Diagnostic lons (m/z)273 mlz 247

100.03548.4100.0PASS


Diagnostic lons (nVz)300 m/z 326

Diagnostic lons (m/z)300 m/z 326

2413.510.3


(,y531.715.0

PASS




01020 t o t)

4/W

zlrt,ln

S

Pos Control

Diagnostic lons (m/z)273 mlz Z4t105085 W1100.0 7.9

43718.3 -1653100.0 5.0PASS PASS

23366 2413.5100.0 10.3

114448.8 8802100.0 7.7PASS PASS

Diagnostic lons (m/z)

105085 8271100.0 7.9


963.5 4031100.0 418.4PASS FAIL


Diagnostic lons (m/z)300 m/z 32623366 241t5100.0 10.3733.8 1561100.0 212.7PASS FAIL

105085 8271100.0 7 .9

12717.7 0


366 2413.5

1q0.0 10.3

,4+c,/r,t\

, C:rXcalibur\...\Negativelon\21635

NL: 6.2085

41-49 RT: 0.78-0.93 AV: 3- c ESI SRU ns2 291.20e15.00 I 2z" 246.50-325.50z Intensity Relacrve

Neg. Control GEDTA blood swab ext.)

2153sil4?-sr nr;l.lllilg-r ev; zFr - c Esl SRM ns2 344.20G15.00 I 2z- 298.00-326.50

z Intensity Relaltve299.70

ofi ?'oIo ,t)

'[-'lvt

02116107 06:53:36

RT:0.93 -M:22116 RT:0.97

AA:47160100.1

*J 272.'t0213.21 98{.3 100.00

-z?s.,// \/ l,tn I( Mv /\-/

/(w

oo

Df

€o

oo

@W

€n q"'N u( rtt)

illlz= 282.8-2U.3 F: - cESI SRM [email protected] |282.7*2U.251 MS2't635

Time tminlTime (min)

02116107 07:26:12 K2 extractC:Xcalibur\...\Negative lon\21 638

z- 298.00-326-50z Intensity Relative300.13 105?.3 LO0.0O

@w

z Intensity Relative246.8L 9{0. o 100. oo

@I\t/'

RT:1.30 NL:1.36E3M: 6867 Nz= 272.1273.5 F: - cI ESI SRMms2

3il:339if 331272.50-273.501 MS

tdz= 246.*217 .5 F: - cESI SRM [email protected] [246.50-217.fi.272.50-273.501 MS21638

':l

I6

€oio

10(

4

I'

7C

55

50

45

40

u'a,lnto ,t:4b(,r')

nvz= 311.$312.5 F: - cESI SRM [email protected] I311.5C.312.501 MS21 638

Tlme (mrn)

C:U(cqllbuA...\Negative lon\2 1 641 02/16107 07:58:57 Q46 extract

aT. n raM:28309 RT: 1.35

AA:18923- c ESI sR!.{ ns2 344.20c15.00 [ 2z- 298.00-326.S0z Inteosity Relative299.'t9 2907. 0 1OO. 00

rot

'lNL: 5.61 E3nlz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.fi,272.sG273.501 MS21il1

1 00-1

^-lJ--l--lolEo-l

I7U'-l70i'^-l"l60-l

JTI

501

4s-lI

oo-l

--l^^l*-j

@

^J\v

@ttllL

d1llil o \?

lWr\*\fl

r/z= 31 1.5-312.5 F: - cESI SRM [email protected] I311.5G312.501 MS21il1

f* r,q"/ t ><t\ Time (min)

C:\XcalibuA...\Negative lon\21 644 02116107 08:31:35

(Jq u

NL:0r]iz= 272.5-273.5F: - cESI SRM [email protected] [246.fi-247.fi,272.50-273.501 MS21644

NL:0

1644#4I-49 RT: 0.78-0.93 AV: 3- c ESI SRM ns2 291.20015.00 Iz- 246.50-326.50

contains no data.

rnlz=246.5-247.5F: - cESI SRM [email protected] [246.*-247.s.272.5O-273.50j MS

oIE

{o

-Eo

RT;0.87AA: 13:104346

NL: 1.24E6nh= 242.8-2U.3 F: . cESI SRM [email protected] MS

(ra,\

RT: 1.20AA: 6655

K3 extract

NL: 1.75H!mfz= 299.$300.5 F:. cESI SRM ms2

13333_9J333.r32s.5G320.501 MS

216441f59-63 RT; 1.12-r.20 ev: 2| - c ESI SRM ns2 344.20015.00 t 2z- 298.00-326.50

Intensj.ty Relative963.5 23.90

4031.0 100.00325.41

4ru\fl

C:D(calibuA...\Negative lon\21 647 02116107 09:04:15 Q47 extraci

NL:0

'n'lz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.50t MS216/'7

;M:RT:AA:

RT:1.19AA:4347

1,81z= 246.50-326.50conlarns no data.

z" 298.00-326.50contains no data.

nlz= 2465-247.5 F: - cESI SRM [email protected]?.fi-273.501 MS

nlz= 282.8-2A43 F: - cESI SRM [email protected] I242.75-2U.25l MS21e47

rn/z= 325.t326.5 F: - cI ESt SRM ms2I [email protected] 299.5G300.5o,I g2s.s0-326.501 MS

I 21u7

I

I

I

I

"lol6lxltlot<lol6t@i-l

I

I

I

I

I

I

NL:2.10E5, nn_ rfz= 31 1 .$,312.5 F: - c'-- I I EStSRMms2,5.1 | iff:B&gllgr".'oJ Il 21u'|

8q llsolll'u'l I I'ol ll'l /l'ol /lssJ iluo.liloul l\oo'l I \

'u'l I \

'o'l I \27 1\2o-l | \lsll

\'ll\'-1/ l.ol-+-1->-+

Time (min)

6t,u,/ t:>5\

"ili:

,ool9H

on-l--lqr--l*l'l,\_-l*l*-]*l*lorloo-l

*l^^lar-l

Time (min)

C:l(galibpr\...\Negative lon\2.1 650 0?/16107 09:36:53 K4 extracl

RT: 1.3A NL:4.52E3M: 22883 n,tz= ZTZ.+213.5 F: - c

NLOrn/z= 299.$300,5 F: . cESI SRM ms2

333:',39Jfi93t325,5S.326.501 MS

Scan contains no data,

@lw

ESI SRM ms2

3il:3391i33t272.50-273.501 Ms216sO

':i

@l,w

@o

o

o

r.4 o r,,0\o\J

0dilst* 44b

rnlz= 246,5-247.5 F: - cESI SRM [email protected] t246.50-247.50.272.so-223.50i Ms21 650

rnlz= 325.5.326.5 F: . cESI SRM ms23/[email protected] t299.50-300.50_ -

325.50-326.s01 MS21650

rvz= 311.$312.5 F: - cESI SRM [email protected] t31r5G312.501 Ms

( ral)

C:U(calibur\...\Negative lon\21 653 02116107 10:09:33 Q48 extract

NL:2.67E3rw2= 299.5-300.5 F: - cESI SRM ms2

t#3381333'325,50-326.50i MS

NL:0||r'z- 272.6273.5F. - cESI SRM ms2291 [email protected] I246.50-247.50,272.50-273.50t MS21653

1-49 RT: 0.7?-0.92 AV: 3c ESI SRM ns2 291.20€15.00246.50-326.50conlains oo data.

RT;1.04AA: 23310

2I 653i|43-ss nr, o. er-il?-iE-a-F: - c ESI SRM ms2 344,20015.00 { 2B,/z- 298 .00-326. 5O

z Intensity Relative300.25 133.8 47,01

1561.0 100.00

@,N

o

.go

NL: 8.53E5mJz= 282.8-2&.3 F: - cESI SRM [email protected] I292.75-2U.25t MS21653

ood

€o

=o

^,afl:)oo"^,'lo'r'

Cu-nt( r"t+\

NL: O

nJz= 246.5-247.5 F: - cESI SRM [email protected] I246.50-247.50,272.sG273.s01 MS21 653

":44J,

C:\XqglibuA...\Negative lon\21 656 02J16107 10:,42:14 Pos. Cont. A (MAL EDTA ext.)

2l656tt4s-49 RT: 0-85-0. 93 Av: 2

z= 246.50-326.50: - c ESI sRM ns2 291.20915.00 t 2 ... NL: 3.25E4

m/z= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.501 MS21 656

r/z= 31 1.$312.5 F: - cESI SRM [email protected] t31'1.50-312.501 MS21656

1656ia51-63 RT:0.9?-1.20 A1 4: - c ESI SR!.i ns2 344.20.a15-OO t 2z= 298.00-326.50z Intensity Relative

23366.0 100.00ZCTJ.5 IU. JJ

RT:0.97AA:549785Intensity Relative

821t.0 1.81r05085.0 100 ,00

300.02

AA: 90037

e

o!ctod6c.

@Ay

Nz= 282.8-28/.3 F: - cESI SRM [email protected] I282.7+2U.251 MS

/t/W

f" +*a(,''ts)

fflz= 246.1247.5 F: - cESI SRM ms2291 [email protected] [246.50-247.50,272.50-273.501 MS21656

'l-ime (minlTime (min)

'.,ill

C:U(qalihuA...\Negative lon\21 659 Pos. Cont. B (Q49 ext.)

NL:2.28E5m,2= 299.S300.5 F: . cESI SRM [email protected] [299.50-300.50,

-

325.50-326.501 MS21659

NL:6.35E4rnlz= 31 1.t312.5 F: - c

l-1RT:0.97AA:2619370

- c ESI SRU nsz 344.20c15.00 I 2 ...z- 298.00-326.50z Intensity Rel.ative299.91 114448.9 1 00. o0326.04 8802.0 1.69

@/w

100-.1

'-l

",18q.o']

zN

'o']65j@ ^^l,. -|

l45-1

40l?6J*lro-]

24,-lril'-l'l

o.26@E

roo-, M'

nr-l

*-lru-]

801

tA

^.]ul*-l*-]*-1orloo-l

rrl

'"]

ESI SRM [email protected] [246.50-24?.50.272.5G273.501 MS21659

1 nlz=282.8-2U.3F:-cESI SRM [email protected] [282.75-2U.251 MS21659

@/1N^

ESI SRM [email protected] I311.50-312.50] MS21659

Q+u,( ,'at'\ f ime (min)

,.';,-i;

662f43-53 RTr O.g1-1.19 AV:6- c ESI SRU ns2 [email protected] I 2

298.00-325.50

02116107 11:47:36 Spot LOD, 1uL Q49C:U(qalibur\...\Negative lon\21 662

nlz=272.5273.5F: - cESI SRM [email protected]

ms2r5.00 [

246.50-247.50,272.50-273.501 . MSa tooz

'NL:5.10E5

dz= 242.8-28,4.3F: - cESI SRM [email protected] I282.75.2U.25t MS21662

RT:0.85AA: 11851E1001

*l

@(tw0

/\1,,"

0.,';:L.f* ++a( r^z\

RT:0.88AA:363506

filz= 246.1247 .5 F: - cESI SRM [email protected] [246.50-247.fi.272.50-273.501 MS21662

oo

o

o45

40

0?/17107 12:20:10 Spot LOD, 2 uL Q49

7.04E4

. C:u(calibud...\Negativelon\21665

- C-ESI SRM ns2 344.20015.00 [ 2z- 298.00-326.50z Intensity Relative3:: !9 286e?.s 100.00r.o.z6 262.5 0.91

0.88746703

' ,.(RT:AA:

04AI^"

rnlz= 282.4-2U.3 F: - cESI SRM ms2

i3l7t9Jfi3t".

^ nrOl)

0'10',Jrr\*6: aa( ,,s)

m/a= 299.$300.5 F: - cESI SRM ms2

133:338J333t325.sG326.501 MS21665

nlz= 246.1247 .5 F: - cESI SRM [email protected] I246.fi-247.50.272.50-273.501 MS21655

I 00-l

*t*-1Ail*iro-1

7l,"1*t60-l

-- |

::l'ul45-1

rc-lI'-t

^^ i

'u-l

r/z= 31 1.5-312.5 F: - cESI SRM [email protected] I3t'1 .50-312.501-MS21665

@4M

@oF

€oio

$,

C:'"'icalibur\data\Brewer\070201 01 3\2'l 601Tfog

02116107 12:03:08

NL: 1.36E3rvz= 159.$'160.5F: + c ESI Full [email protected] [ '12s.00-315.001 MS2160'l

10€

95

90

80

70

I 0o6uoo

-go

66J--61 NL: 2.83E59.04 TtC MS 21601

3044.'15

2403.28

3544.U

cua 6zt6.93 510 E.Ss

tnlT- 246.5-247.5F: + c ESI Full [email protected] [125.00-315.001 MS21601


+ c ESI Full ms2 [email protected] [ 125.00-315.001

nxnrnrT 50005 cF 381

oll;l,a3'M{\',

C:)XcalibuAdata\Brewer\O7020 1 0 1 3\21 602r, t.

cDP ozrcrc7 i2:14.29

NL:0mrz= 159.5-160.5F: + c ESI Full [email protected] [125.00-315.001 MS21eo2

. a nqEr

100-l

*lnol

65t

.o-]I

,o-lI

ru-i

,q ^n-l

m/z= 246.5.247.5F: + c ESI Full [email protected] [125.00-315.001 MS21602

6u('il)

Neg. Control (-EDTA blood swab ext.)

160?#65 RT:o.EE AV: 1 NL: 7.25E3: + c ESI Full ms2 [email protected] [125.00-315.00]

@41,/

C:VcalibuAdata\Brewer\O70201 O 1 3U1 603-rg

-

0?/16107 12:25:21

NL: O

nvz= 159.$150.5F: + c ESI Futl [email protected] 25.oo-5i s.ool' Ms21603

rnlz= 246.$247.5F: +cESl [email protected] Ms2l 603

3.43E3

.t onEE

Ttc {\rs 21603

oo

0

Eo

t"qK

BLANK (neg btood, Dt H2O ext.)

JUJrcO A I : U.OO AV: 'I NL: O+ c ESt Fuil ms2 [email protected] [ 125.00-315.001

@M

C:Xcalibur\data\Brewer\07020 1 Ol 3U 1 604f\

-lo6'0A16107 12:36:16

:1.1gEsTIC i/ls21604

oooE

o.:oo

ti+

rnlz= 246.5-247 .5F: + c ESI Full ms2

?33339f333rr^

/ta)

BLANK (neg blood, Dt H2O ext.)

: + c ESI Full ms2 [email protected] [ 125.00-3iS.0OI

@/1/y

C$(calibur\data\Brewer\07020 1 01 3U l 605\-

7.U

NL:0m/z= 159.5-160.5F: + c ESt Full [email protected] |125.00-315.00t MS21605

ntlz= 246.5-247.5F: +,: ESI Full [email protected] [125.00-315.00t Ms21605

JDP' 02116107 12:47:04

NL: 9.45E4Ttc Ms 21605

oo

E

o.z-g!o

5* 4+,(rv\

K2 extract


@Aw

C:\Xcalibur\data\Brewer\070201 01 3121 606rl -|vg' 0U16107 12:57:54

: 2.81E3

100-l

ru-.1

ro-l

*lro-l

to-]I--l

I ^^-.1

ftlz= 246.5-247 .5F: + c ESI Full [email protected] I125.00-315.001 MS21606

m/z= 159.5-'160.5F: + c ESt Full [email protected] [125.00-315.001 MS21606



@A/^/

C',Wcaliburtgata\Brewer\070201 01 3U1 607 J DI'02116107 01:08:5'l

NL:0rn/z= 159.5-160.5F: + c ESI Full [email protected] Ms2',t607

m/z= 246.1247.5F:+cESl Fullms2293 [email protected] [125 00-315.001 MS21607


: + c ESI Full ms2 [email protected] [ 125.00-315.00]

@^N

C:Uftalibur\datia\Brewer\070201 0 l 3U1 60g'l

NL:0rvz= 159.5-160.5F: + c ESI Full [email protected] I12s.00-51s.oot'Ms21608

2493.40

239

,L++


@/vw

C:\XcalibuAdata\BreweA070201 01 3\21 609

nlz= 1 59.5-'160.5F: + c ESI Futl [email protected] t125.00-31 5.001'MS21 609

'NL: 0.r z=246.1247.sF: + c 951 PrU r.,[email protected] t1 25.00-31 5.00t-Ms21509

,{r v


;;Esr i;il 'U 2r!.bb61';:ddr 125.00-315.001

@4/


+ c ESI Full ms2 [email protected] [1z5.oo-315.00]

fre\oyAl,/

l{y t1,

-C:U(calibur\data\Brewer\07020'l 01 3\21 6.1 .l t op o2t16to7 o1:52:18

NL;0nvz= 159.5-160.5F: + c 551 Pu1, tr,[email protected] [125.00-315.001 MS21611

100-l

ru-]

e0-j

e*].o-l

^-lto-]

uuJ

P ^n-j

ti+

5086.94497433

5.U

5.12

J I rruJ ^ t. u.oo Av: I NL: u

+ c ESI Full ms2 [email protected] [ i2S.O0-315.001

@Al,/

C:U(calibur\datia\Brewer\070201 0 1 3\2 1 6 1 2"--_ ffip oa$rc7 o2:03:10 BLANK (neg blood, Dl H2O ext.)

Full ms2 293.00@1S 00 [ 125.00-315.00]

10(

oa

8C

/a

70

6o

a

ooo

@A/N

NL:3.196E5Trc Ms21612

4255.8't

^^^lJOO I

t-uV

o

C:,\XcalibuAdata\BreweA07020't 013U1 6l 3

N!: onVz= 159.5-160.5F: i c ESI Full [email protected] I125.00-315.00t MS21615

1 00-l

*-]*.1uu-l

801

zs']

toJ

5s-l

I

i. -"-Jol3 4s-lol.9 40-.1-^,1

I

ro-]

ru-j

,olru-l

ro-]

-l

mlz= 246.1247.5F: + c ESI Full ms22e3 [email protected] I12500-315.001 Ms

702


: + c ESI Full ms2 [email protected] 1 ,|ZS.OO-atS.OOJ

@

^W

og

C:U(calibur\data\Brewer\070201 O1 3U 1 61 4'i

drp 02116107 02:24:52

7.94E3

NL:0rn/z= 159.$160.5F: + c ESI Fult ms2,o? nn6la

^n r

12s.00-315.001 Ms21614

100

90

85

80

75

70

65.

rnlz= 246.5-247.5F: + c ESI Full ms2

ir,ifl3.sl833,r^

oooE

o€6

NL: 3,86E5Ttc t,ts 21614

Q47 extract

+ c Est Futi mii 2s's.bb@idno"i 1z5.oo-31s.001

@I\IIP

- C :U(calibur\data\BreweA070201 0 1 3U 1 61 5t \., + 02116107 02:35:44 BLANK (neg blood, Dl H2O ext.)

NL:0rn/z= 159.$160.5F: + c ESI Full ms2,ol nn^a E nn I12s_00-315.001 MS216'15

oAlp

li,t,t

C:lKcalibuAdata\Brewer\070201 0 1 3U 1 61 6 frF 0?/16107 02:46:33

NL: 0nvz= 159.5-160.5F: + c ESI Full [email protected] [125.00.315.001 MS21616

tnlr-246.U247.5F: + c ESI Full [email protected] [12s.00-315.001 Ms216'16

1.70E3

o,:.g!o

ooo

o

.go

1.33E5Tlc lls 2'1616

ti+



t00

@N,lv

C:\)(calibur\data\Brewer\07020 1 0'l 3\21 61 7 02116107 02:57:25

NL:0r/z- 159.5.160.5F: + c ESI Full [email protected] ['125.00-315.001 Ms21617

fiilz= 246.5-247.5F: + c Egl Pu11 t.,[email protected] {125.00-3'15.001 MS2'1617

1.76E5MS 21617

ooo

aoo.:oo

tit +/r rt

K4 extract

01 /fft5 r{t: 0.66 AV: I NL: 5.63E3+ c ESI Full ms2 293.00@ t5.00 [ 125.00-315.00]

@Aj,P'


i c ESI Full ms2 [email protected] [ i25.o0-3i5.ool

C:Vcalibur\data\Brewer\07020101 3\21618 :floyg 02t16t07 03:08:17

rn/z= 'l59.$.160.5F: +cESl [email protected] [125.00.315.001 MS21618

1001

ru-l

ro-1

ro-]I

ru-l

70-J

^.-l--lI "n_l

C.:\Xcalibur\data\Brewer\070201 01 3U 1 6 1 9 fttF o2t16tot o3:1e:12 BLANK (neg blood, Dt H2O ext.)

NL:0nvz= 159.5.160.5F: + c ESI Full ms2,ol nn6r a nn r

125.00-315.001 MS2't619

10(

oa

80

70

rrlJz=246.5-247.5F: + c ESI Futl ms2

?:33393#rr^

A AOEt

: {./ /ECTtc Ms 21619

oo€E

foo

-=6dtr

tr'/

i ; ; l-sl ini '-ii zg'g.bbtb iiio' r I 2s.00-3 I 5.00I

@AtN


@,/\Ilv

C:\Xcalibur\data\Brewer\070201 0 1 3\21 620tL

fi4 oz16to7 o3.29:s7

NL:0nvz='159.$'160.5F: + c ESI Full [email protected] [125.00-315.001 MS21620

laa7.90

o

;

E

C:U(calibur\data\BreweA070201 0 1 3\21 621_ T-ry 02116107 03:40:49 BLANK (neg blood, Dl H2O ext.)

NL;0rvz= 159.5.160.5F: + c ESI Full msa

!i!1{38r33&',.

: /./cEJ1001

nlrol

"-lro']

tulto-l

6sir -^-l

rnlz= 246.9247 .5F: + c ESI Full [email protected] [125.00-315.001 MS21621

oo6

o.:-s!o

flc Ms21621

fl,^ 3ll

%,{+ v


/t , /tt

C:D(calibur\data\BreweA070201 0 1 3U1 622 {n(t 02116107 03:51 :42 BLANK (neg blood, Dl H2O ext.)

NL:0m/z= 159.$160.5F: + c P51 Pr11 [email protected] [125.00-315.001 MS21622

Z.OJEJ8.40 mh=246.5-247.5

F: + c ESI Full [email protected] [125.00.3'15.001 Ms21622

NL: 4.i'1E5rc Ms21622

oo

o'aoo

3915.35

| 427I 5.84 5'18

7.09 546

209z.w20s

5JZ7.28

3.?2

lttzzfttt t{t: u.66 Av: 1 NL: 1.13E4: + c ESI Full ms2 [email protected] [ 125.00-315.001

54

38

36

34

@rus

C:U(calibuAdata\Brewer\07020 1 01 3\21 623

4.42

02116107 04:02:32

NL:1.33E5n/z= 159.5-160.5F: + c ESI Full [email protected] [125.00-315.001 MS21623

oo6

o

oE

Ttc Ms 21623

419 4755.72 6.49

Lg-

Pos. Cont. A (MAL EDTA ext.)


?oJ.hoL,M

\,$v

Q:U(calibuddata\Brewer\070201 01 3U1 624 d"$ 0U16107 04:13:22

NL:0nvz= 159.$160.5F: + c ESI Full [email protected] [12s.00-315.001 MS21624

'NL: 6.06E3nlz= 246.5-247 .5

100-l

^-l"l6J*tqEl*t80J

I71)

.^l^_lol

l

6218 le ees

F: + c ESI Full [email protected] [125.00-315.001 Ms21624

NL:4.63E5Ttc Ms21624

I.z.go

5.El407 l4s.56 lJ4.0€

,/l c -i


324#65 Rr: O.E6 AV: 1 NL:0+ c ESI Full ms2 [email protected] [125.00-315.001

@/W

C:Xcalibur\data\Brewer\07020 1 01 3U1 625 0?/16107 04,'24:14

rn/z= 159.5-160.5F: + c ESI Full [email protected] I125.00-315.001 MS21625

tlz= 246.5-247.5F: + c ESI Full [email protected] [125.00-3'15.001 Ms21625

4.54E3

4.97E5Ttc MS 2'1625

oo

oo

o-

4.1

2893.95

ssg | | 9.298.19 ll I

4/ t<,


1625#€5 RT:0.E6 AV: 1 NL: 2.9EE3: + c ESI Full ms2 [email protected] [ 125.00-315.00]

@}IM



@M

teV 0U16107 04:35:06

1 00-l

*trol*l"-l75-l

-^l

^:--l

C:XcalibuAdata\Brewer\070201 01 3\2 1626 () o " u) TbF oa't6n7 o4:35:06

NL:1.08E5rdz= 159.$160.5F: + c ESI Full [email protected] [125.00-315.001 MS21626

fflz=246.5-247.5F: + c ESI Full [email protected] [125.00.315.001 MSztozo

{"+/;<


1

+ c ESI Full ms2 [email protected] [125.00-315.001

@A^jl'J


+ c ESI Full msz 293.00@ 1 5.00 [ 125.00-31 5.00]

@ffN

-ID$ 0A16107 04:45:57

n/z= 159.$160.5F: + c ESI Full [email protected] [12s.00-315.001 Ms21621

NL:1.23E4rnlz= 246.5-247.5F: + c ESI Full [email protected] ['125.00-315.001 MS21627

1001

s5-.1

on-l*l"-l

"n-l;L'-l7o-l

I

--to --l

o

o

€!

o6E

o.Jz6468.84

I

624 |

8.54 I

azJ7.24

4.66E5Ttc Ms 21627

zsz i6^3^ a'Ps

Co+

C:Xcalibur\data\Brewer\O7020 1 01 3U 1 628 ',w 02116107 04:56:49

NL:0r/z= 159.5-160.5F: + c ESI Full [email protected] I125.00-315.00] MS2162A

ooG

o.:6o

@

Tlc Ms 21628

,{* q/ i1'7


+ c ESI Full ms2 [email protected] [ 125.00-315.00]

C:U(calibur\data\Brewer\070201 01 3U 1 629

309

4.03 |

zJo

taq

OA16107 05:07:38

NL: 5.73E3r/z= 159.t160.5F: + c ESI Full [email protected] Ms21629

rlz=246.1247.5F: + c ESI Full [email protected] [125.00-315.00] MS21629

1 001

ss-J

ro-l

ru-l

:tr

"-]zo-l

651

P -".1

o

-Eo

ooop

o,:6E

AA?NL: 5.1 6E5Ttc t\,ts 216295.46

i ros4.503091 | 7.68

^o99

2.1

Spot LOD, 1uL Q49


@Atrr

C :U(calibur\data\BreweA07020 1 01 3\21 629I

Spot LOD, 1uL Q49

1629F64-O5 t{t: 0.6/{t.69 AV: Z NL: 4.35EJ: + c ESI Full ms2 [email protected] [ 125.00-315.00]

::r

4*luo-]

'-tro-1

65-l

-"1I,..]

0.64

A/'r

@N

{+q

0.75

,rril'\/4/t <,

C:\jt(calibur\data\Brewer\070201 01 3U 1 630a . e

-Jnp 02/16/07 05:'18:30

NL:2.02E3rvz= 159.$160.5F: + c ESI Full ms2z5J.W@ tC.UU I125.00-a15.OOl'MS21630

100-

*-]

10c

9€

85

EC

r!70

ooo

a0o

.Eotr

228211 3.12

o5.Eo

: 7.1 1E3n122246.1247.5F: + c ESI Full ms2293 [email protected] [12500-315.001 MS2't630


+ c ESI Fuil ms2 [email protected] [ 125.00-315.00]

@Af\N',

C :U(calibur\data\Brewer\070201 01 3Ul 6314..

1 00f^-l"-l

:Ivp 0A16107 05:29:22

NL: 1.42E3nvz= 159.5-160.5F: + c ESI Full [email protected] I125.00-315.001 MS21631

{u tt|/ t,-t


031t65 RT:0.88 AV: 1 NL: 1.0384+ c ESI Full ms2 [email protected] [ 125.00-315.00]

@r1|\/

C:Xcalibur\data\BreweA070201 01 3U1 632I =---

'05o<J*t67

0.91

,ra 356i.;; 4.s6

f,DF 0U16107 05:40:13

NL: 1.27E4rn/z:159.$160.5F: + c ESI Full [email protected] [125.00-315.001 MSztoJz

1001

'-loJ*l*-]ro-l

tr-]to-l

*i'-l

1orloo-1

^-l,"-.1

ro-l

'1,o-.1

tq!'-l1 0-1

-l

mlz=246.U247.5F: + c ESI Full [email protected] MSz toJz

:4,25E3

: c.u/ E5Ttc Ms21632

{" v.lu/,, -F

461 876618 zY.'eE 561

JOZ

Spot LOD, 2 uL Q49

Z IOJMO X I ; U.YU AV: 1 NL: g.Z/E3F: + c ESI Full ms2 [email protected] [ 125.00-31S.00]

. C:U(calibur\data\Brewer\070201 01 3\2t 632 (2.:v^a ) ar\ 0416107 05:40:13

: 2.30E5Trc Ms 21632

b

oo

f

o6o

fn

NL:127E4nvz= 159.$160.5F: + c ESI Full [email protected] [125.00-315.00t MS21632

NL: 3.51 E3.r,lz=246.5-247,5F: + c ESI Full [email protected] [125.00-315.001 MS2'1632

Spot LOD,2 uL Q49

r oozrco n t ; u.vu Av: t NL: 9.2/Eo: + c ESI Full ms2 [email protected] [ 125.00-315.00]


+ c ESI Full ms2 [email protected] [ 125.00-31S.OO]

@AI\}.v

C:\,Xcalibur\data\Brewer\O7020 1 01 3\21 633 l-s oF 02116107 05:5't:09

m/z= 159.!160.5F: + c ESt Fult [email protected] Ms21633

1001

ro.l

,A ot.L*ll|l^.ll^ll,ll

o *ll

279 3443.81 4.70

2U

a

C:'XcalibuA...\Negative lon\21634 A70Zol 0 t3 j-oF02116107 06:42:35 BLANK (neg btood, Dt H2O ext.)

NL:0nlz= 272.5-273.5 F: - cESI SRM [email protected] t246.50-247.50.'272.50-273.soi Ms2163/

NL:4.52E3trlz= 246.$247.5 F: - cESI SRM [email protected].'272.so-273.s0i Ms2163/

m/?= 325.5-326.5 F: - cESI SRM ms2

133339J,133r325.50-326.s01 MS

8oE

"Eo

@n^iL

r/z= 31 1.5-3i2.5 F: - cESI SRM [email protected] I31 1,50.312.501'Ms2163/.

nlz= 282.t1-284.3 F: - cESI SRM ms2

lSiiS.gJfj$r",

C:\Xcalibu^...\Negative lon!21635 070/.O I Ols 02116107 06:53:36 Neg. Controt (-EDTA blood swab ext.)

100rI*l

-"1--

NL:2.68E3nlz=272.5-273.5 F:. cESI SRM ms229'[email protected] [246.50-247.50.272.50-273.50i MS21 635

rn/z= 299.5-300.5 F: - cESI SRM [email protected] I299.50-300.50.-325.50-326.501 MS21635

@/\,P

o

@

o

AtIt/

ffi,v

/Tr'z= 246.1247.5 F: - cESI SRM [email protected] t246.50-247.50,272.50-273.s01 Ms21 635

ntz= 282.8-28/..3 F: - cESI SRM [email protected] I282.75-2U.251 MS2'1635

100-l

*l*.185-J

'o-ltu-l

1lor-l

uo-J

*luo-]

ou-l

oo-]

ru-]

rol

ntuv

C:D(calibur\...\Negative lon\2 1 636 e7ozotol3 Jop 0?J16107 07:04:28

f.vqa/'t, z


%

rvz:299.$300.5 F: - cESI SRM [email protected] t299.50-300.50.'325.50-326.50i MSz toJo

tol

'lno-J

ru-l

80'j

zs-]

zo]^-lol

s oo-]clo

€@

@

nlz=246.5-247.5 F: - cESI SRM ms2

lil:33.91f 33t272.s0-273.501 MS21636

rn/z= 282.8-2U.3 F: - cESI SRM nrsz

l3l?&gJfi3'r",21636

rvz= 325.5-326.5 F: - cESI SRM msz

3d3339J333r325.50-326.501 MS

ANW

C:Xcalibur\...\Negativelont21637 077LOlO13 J'lp 0?/16107 07:15:23

NL:0flilz= 272.5-273.5 F: . cESI SRM [email protected] l246.50-247.50,272.s0-273.501 MS21637

BLANK (neg btood, Dt H2O ext.)

1001

sslro-l

ru'l

ro-l

"-l,o1

*-1

I 60-l

fitlz= 282.8-284.3F: - cESI SRM [email protected] I282.7s-2U.251 MSltoJt

8d

o

-qo

, oo-]

*ls0-1

es-]

Eo-]

ruJ

70J

.s-]

.o-]-- |*l*-l4s-..1

."]^-l"'-l3q,u)

I

20i,

''-]ro-]

F

NL:4.16E3rn/z= 31 1.$,312.5 F: - cESI SRM [email protected] I31 1 .50.312.50t' MS

frt 4,/r./,, u\

C:D(calibur\...\Negative lon!21638 A7 OLl I o I A -tD p 0?16107 07:26:12

,o5e$l

NL: 1.36E3rnlz= 272.5-273.5 F: . cESI SRM ms2291.20@15,00 [246.50-247.50,272.s0-273.501 MS21638

4.04E3ftlz= 246,5-247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.s01 MS2'1638

fflz= 282.&2U.3 F: - cESI SRM [email protected] [282.7r2U.251 MS21638

nvz= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.501 MS21638

q1001

nl*-l

:fi:1,"-l

'luo-]

--l-^l--lou-j

40-J

^-l*l30-l

I

8.73E4m/z= 31 1.5-312.5 F: - cESI SRM msz3s6.00@ 1 5.00 [311.50-312.501 MS21638

{ur 4(

Q:U<calibur\...\Negative lon\21639 01A7Ol 0l 3 JTP 02116107 07:37:08 BLANK (neg blood, Dl H2O ext.)

NL:0rnlz= 272.5-273.5F: . cESI SRM msZ291.20@'t5.00 |246.50.247.50.272.50.273.501 MS21639

r lz=246.5-247.5F:-cESI SRM [email protected],272.50-273.501 MS21639

m/z= 325.5-326.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MS21639

m/z= 311.5.312.5 F: . cESI SRM [email protected] [311.50-312.501 MS21 639

@4,ur'

8c

o

.Eo@

Aw

rr'z= 282.9-2U.3 F: - cESI SRM [email protected] I282.75-284.251 MS21639

1 001

--l*-l--t*l80-l__l, "-l

ro-j

rul*-l*i*lou-]

,o-l

*l.v-1

I

1.'i[+q

./'l1

4[v

C:\XcalibuA...\Negativeton\21640 C70Z0l0lJ 16p 0?J16t07 07:48:03 BLANK (neg blood, Dt H2O ext.)

@n0t"

6

@

.p

NL:0tr]/z=272.5-273.5 F: - cESI SRM [email protected],272.50-273.501 MS21640

NL:9.94E3n/z= 299.5-300.5 F: - cESI SRM ms2

133339J333r32150326.501 MS

m/z= 325.5-326.5 F:. cESI SRM [email protected] I299.50-300.50,325.50-326.501 MS216/0

1.05E4NL:0nlz= 282.8-284.3 F:ESI SRM ms2 nVz= 31 1.t312.5 F: - c

ESI SRM [email protected] MS21 640

[email protected] [2?21s-2u.2sl Ms

{* aatt /lr

At\lv

NL:5.66E3nvz= 299.$300.5 F: - cESI SRM [email protected] I299.50-300.50.'325.50-326.501 MS21641

rr'z= 246.5-247 .5 F: - cESI SRM ms2291 [email protected] I246.50-247.50,272.50-273.501 MS216/.1

C:tXcalibur\...\Negative ton\21641 0l0LOl p 13 a6p 02116107 07:58:57

NL: 5.61 E3rlp 272.5-273.5 Ft - cESI SRM [email protected] [246.50.247.50,272.50-273.501 MS21€/1

| 001

95-..1

"l

NL:2.19E3n/z= 325.5-326.5 FESI SRM [email protected] [299.50-300.50,325s0-326.501 MS

^KlL'r '.\,('r.iD

t ti I L /, ttl uv@

nru^1

NL: 8.52E:5fiilz=2828-2U.3F'. - cESI SRM [email protected] I282.75-2U.251 MS21€/1

100-.]

ru-l

'o-l*-lultu-1

70-..1

",]n ^o-l

*"1I

:l*lrnl--l'-l,o-.1

ru-l

,o-]

5!

o11 001

*lSJ

^-lo"-l

*-l

::l,"1^-l"'l60J-- |*l*l45-1

oo-l

as-..1

r-lI

A\1^',

C:\Xcatibur\...\Negativeton\21642 OlLLOl0lJ Jnl 0?/16107 08:09:50

trvz= 325.5-326.5 F: - cESI SRM [email protected].'325.50-326.501 MS21d42


@,/r{

oo6

€@

.go0

nv

rnlz= 272.5-273.5F: . cESI SRM [email protected] [246.50-247.50.2z2.so-273.50i Ms216p2

5,r (4,

1 00-

'JI,olru-l

80-l

t*lI

to-l

-l8 eo-l

m/z= 246.5-247.5F:. - cESI SRM [email protected] I246.50-247.fi.272.s0-223.50i Ms21642

rnlz= 282.5284.3 F: . cESI SRM [email protected] [282i5-2U.251 MS

0J1001

95i

*_l*-lso-l

ruJ

70!,

^-loc-

.o-]I

s5-J

so-l

ou-l

oo-l

ru-1

"-l

/'rA z\

C:u(caliburl...\Negarive lon\21643 0T0Zo/ot3 lTp 02116107 08:20:45

m/z= 299.5.300.5 F: - cESI SRM [email protected]

I299.50-300.50.'325.s0.s26.50i MS216/3

rtlz= 246.5-247.5 F: - cESI SRM [email protected] [246.fi-247.50,272.50-273.501 MS21643

@r$/

s.89E3nlz=282.8-2U.3'F:, - cESI SRM [email protected] [282.7*2U.251 MS21€/.3


m/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.501 MS21€/3

@^N

C:lXcalibur\...\Negativeton\21644 0ZoZolo/3 JDB 0?/16107 08:31:35

Nz= 272.5-273.5F: - cESI SRM ms2

ill:339ii33,t272.50-273.501 Ms

rrvz= 246.$247.5 F: - cESI SRM [email protected] I246.50-247.50.-zzz.so-zz:.soi tr,ts2'tu4

K3 extract

rvz= 299.5-300.5 F: - cESI SRM ms2

133:33€J333t325-s0-326 501 MS

%1.24E6

*{}

od

o

@o %

1.09E5rdz= 282.t]-284.3 F: - c

:3!?39;figr".

,Y4

rvz= 311.5-312.5 F: - cESI SRM [email protected] I311.50.312.501 Ms

/'t'?.

J\I},

C:U(calibuA...\Negative ton\21645 01 0L0 i O 13 Tnp 0U16107 08:42:24 BLANK (neg blood, Dt H2O ext.)

NL:0mtz= 272.5-273.5 Fi - cESI SRM [email protected] I246.5G247.50.'272.50.273.501 MS216/5

rn/z= 299.$300.5 F: - cESI SRM ms2

!i3:338J'133t

!ffi-ezo.sot us

@nN

oo

E

o

oo

@AI.J

5y:4a

trlz= 246.*247.SF:. cESI SRM ms229',[email protected] MS2't 645

, tot2m/z= 325.5326.5 F: - cESI SRM [email protected] t299.50-300.50.-325.50-326.501 Ms216/.5

m/Sz= 282.&284.3 F: - c

;if,3.gJ."'3lr^

nVz= 311.$312.5 F: - cESI SRM [email protected] I311.50-312.501'MS21645

C:Uftalibur\...\Negative lon\21646 070LO t Ol3 frg 02116107 08:53:19 BLANK (neg blood, Dt H2O ext.)

100-lI

J3l

."1-

NL: 4.51 E3NF272.5-273.5Ft - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MS216/,6

NL:6.52E3rn/z= 299.5-300.5 F: - cESI SRM msz344.20@1s,00 I299.50-300.50.'32s.ss326.50i Ms216/6

: 4.2'1E3mlz= 246.5-247 ,5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS2't646

NL: 9.77E:3

mlz= 282.8-28/..3Fi - cESI SRM [email protected] [282.75-2U.251 MS21€,!6

4*b

nvz= 3'l1.5-312.5 F: . cESI SRM [email protected] I311.s0-312.501 MS21646

@Alt'"

oIo

{oFgo0

r*/

10(

65

75

7A

65

OU

55

4n

45

40

30

z,t ^I\J'p

02J16107 09:04:15 Q47 extractC:\Xcafibtlr\...\Negative lon\2,|647 Al|Lot ol3 ftA

rvz= 299.5.300.5 F: - cESI SRM [email protected] I299.50-300.50,'325.5G326.501 MS21647

rniz= 325.t326.5 F: . cESI SRM [email protected] [299.50-300.50,325.50-326.50t MS21647

@tv

@flv

NL: O

f,tlF 272.+273.5F: - cESI SRM [email protected] MS21€/7

m'lz= 246.5-247 .5 F: - cESI SRM [email protected],272.50-273.501 MS21647

C;iXcalibuA...\Negative lon\21648 0702o/ Ot? ftp 02J16107 09:15:08 BLANK (neg btood, Dt H2O ext.)

1001

nu-J

*-l

'lro-l

75-l

?o-l

6s-l

8 oo-l'l

NL:0rj/z=272.5-273.5F: - cESI SRM ms2291 [email protected] r246.s0-247.50.'272.50-273.s0t Ms216/.A

mE= 246.5-247.5 F.. - cESI SRM [email protected] t246.so-247.s0.'272.50-273.501 MS216/.8

n,lz= 282.9-2U.3 Fi - cESI SRM [email protected] I282.7U2U.251 MS

[" q'/

NL:0rilz= 299.1300.5 F: - cESI SRM [email protected] MS21&t8

rvz= 325.5-326.5 F: . cESI SRM [email protected] r299.50.300.s0.'325.s0-326.501 MS21il8

wo

o

@

oo@

nN'

: 7.49E3rvz= 31 1.S312.5 F: . cESI SRM [email protected] Ms

/,nn\

f'ftl,/

BLANK (neg blood, Dt H2O ext.)C:U(calibur\...\Negative lonl21649 CI7oLol OIZ 6g 0A16l07 09:26:04

NL:8.15E2rrllz= 272.5-273.5 F: . cESI SRM [email protected] [246.50-247.50.272.50-273.501 MS21€.4.9

2.3183

'iil

t.F Psiit*1f;L:'jt s t''"

| [email protected] [email protected] [246.50-247.50,27250-273.s01 MS

1001

,5-l

e0-J

*-l80-..1

t;

^]6qI *-]

@Not

ao

.Eo

@nr/

rol"-lo^J--l^-l""1ro-1

trJ

1t::ro"l*lqnJ*loul

ool

*lro-1

illz=282.8-284.3F: - cESI SRM ms2303.20@ | s.00 I282.75-284.251 MS2'tu9

C:\j(calibur\...\Negative ton\21650 o70Zc-> /0 | j -I6p 02/16/07 09:36:53 K4 extract

NL:4.52E3.tl/z=272.5-273.5 Fi - cESI SRM [email protected] [246.50-247.&,272.50-273.501 MS21650

NL: 4,31E3 .-rvz= 299.5-300.5 F: - cESI SRM [email protected] l299.50-300.50.-325.50-326.501 MS21550

tr/z= 325.5-326.5 F: - cESI SRM [email protected] [299.s0-300.50.325.50-326.501 MS21650

1 00-1

o^J*l^n-l

%o

o

€o

6o-

,{\vnf*

o!ol-l

: 1.07E5100-l

*t6!*l*lro-l

tulrol*l60i-- |

".-l5Ui

OJI

oo-]

*l'o-]

rniz= 311.5-312.5 F: - cESI SRM [email protected] [311.50-312.501 MS21 650

L,,t

rl]/z=246.5-247.5F: - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MS2't 650

4+,qO,\1

C:U(calibuA...\Negative lon\21651 O7oZ4l C | 3 TTB BLANK (neg blood, Dl H2O ext.)

@nM'

G

c

oo@

0^^/

0?i16107 09:47:49

NL:0rnlz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-217.W,272.s0-273.501 MS2't65'l

9.39 NL:3.26E3ftVz= 299.5.300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.sot MS21 651

m/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MS21 651

trVz= 31 1 .$312.5 F: - cESI SRM [email protected] [311.s0-312.501 MS21651

qqq.(r\ I

1,t

m'lr-246.*247.5 Ft - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21651

C:\jXcalibuA...\Negative lon91 6 52 0 7 aZ a t o 13 frg 0?J16107 09:58:44 BLANK (neg blood, Dl H2O ext.)

NL:8.85E3rnlz=272.5-273.5F: -cESI SRM [email protected] [246.50.247.50.272.50-273.501 MS21652

nr/z= 299.5-300.5 F: - cESI SRM [email protected],325.50-326.501 MS21652

r/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.50t MS2't652

nvz= 311.S312.5 F: - cESI SRM [email protected] I311.50-312.501 MS21652

:2.55E:lttlz= 246.U247 .5 F: - c

@.oo

!

o

6@

0^r

ESI SRM [email protected] [246.fi-247.50,272.50-273.501 MS21652

C:U(calibur\...\Negative lon\21653 OToLo lo tJ TOp 02116107 10:09:33 Q48 extract

NL:0nnF 272.+273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.s01 MS21653

rnlz= 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.s0-273.501 MS21653

NL:2.67E3rvz= 299.5-300.5 F: - cESI sRM ms234420@'15.00 [299.50-300.50,325.50-326.501 MS21653

NL: '1.29E5

rVz=311.$312.5 F: - c

-'

o

ao

go

s0rg

ESI SRM [email protected] {311.50-312.501 MS,IAEt

m/z= 325.$326.5 F: - cESI SRM [email protected] [299.50-300.50,325.s0-326.s01 Ms2'1653

qqbcrA

C:XcalibuA...\Negative lon\21654 OTOZOI O tg w 02116107 10:20'.25

NL:0tr,lz= 272.5-273,5 Fi - cESI SRM [email protected] [246.50-247.50.272.50-273.s0t MS21654

mlz= 246.5-247.5 Fi - cESI SRM [email protected] [246.50-247.50.272.50-273.50i MS21654

rnlz= ?42.9-28/..3 F: - cESI SRM [email protected] I282.75-284.25t MS2'1654


NL: 7.30E3nvz= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MS21654

NL:3.87E3m/2= 325.5m/2= 325.5-326.5 F: - cESI SRM ms2

%oo6E

aogo@

Al.}"

[email protected] I299.s0-5oo.so.'32s.s0-326.s01 Ms

A. rt{,.]Z', r.q\ ]

C:U(calibur\...\Negative lon\21655 OToLOl A B {f p 021'16107 10:31:22 BLANK (neg blood, Dl H2O ext.)

1 00-

"J*l'1J

NL:3.11E3.r'lz= 272.5-273.5 F. - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MS21655

: 4.05E3ftilz= 246.+247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21655

.r.lz=282.8-2E/.3F'. - cESI SRM [email protected] [242.75-2U.251 MS21655

ll*,/v

NL: 1.57E3r/z: 299.5-300.5 F: . cESI SRM [email protected] [299.50-300.50.325.50-326.50t MS21655

n/z= 325.5-326.5 F: - cESI SRM [email protected] I299.s0-300.50.325.50-326.501 MS21655

2.41e3

|.04E4

%E

@

-ao@Ay

r/z= 311.S312.5 F: - cESI SRM [email protected] [311.50-312.s01 MS21655

(l,gr"\ I

Al\l'I,

C:XcalibuA...\Negative lon\21656 oaoLolol 3 JDp 0?/16107 10:42:14

@AM/

100-l

"-lq8s-..1

*.1I'l

ro-l

*l8.1

iool t it"'lI'tl

NL:1.29E5nlz-272.1273s F: - cESI SRM [email protected] [246.50-247.50,272.5S273.501 MS21656

8.1 0E3n{z= 246.5-247.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21 656

7.0185tuz= 282.8-2U.3 F: - cESI SRM [email protected] [282.7U2U.251 MS21 656

Ic

eo

@

o

€ol*130-J

l

2s1I

,lr qq5--lo ( t,gz

Pos. Cont. A (MAL EDTA ext.)

@N

NL: 3.25E4r/z= 299.5.300.5 F: - cESI SRM [email protected] [299.50-300.50.325.s0-326.501 MS2't655

rvz= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MS21656

5.21E4r/z= 311.4312.5 F:. cESI SRM [email protected] I311.5e312.501 MS21656

C:U(calibuA...\Negative lon\21657 OTaLolOlS JD6 0?/16107 10:53:13

NL:4.56E3NF272.5-273.5F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21657

:2.15E3Irl/F246.+247.5F:-cESI SRM ms22e1 [email protected] [246.50-247.50.272.50-273.501 MS21657

.n/z= 282.8-2U.3 Fi - cESI SRM [email protected] [242.75-2U.25t MS2'1657


1 00-l

rul^n_.{

NL:1.18E3rn/z:299.5.300.5 F: - cESI SRM [email protected] [4W.CU-JUU.JU,325.50-326.50t MS21857

r/F 325.t326.5 F: - cESI SRM [email protected] [299.5G.300.50.325.5G326.501 MS2'1657

@Alv

@

Eo!c

o

.go&

Time (min)

C:XcalibuA...\Negative lon\21658 07 aZol e B T-OF 021'16107 11:04:07

NL:0ilz= 272.5-273.5 F: . cESI SRM [email protected] [246.fi-247.fi,272.50-273.501 MS21 658

filz= 282..*2U.3F: - cESI SRM [email protected] [282.7r2U.251 MS21656

,{* qr/


1001

oR-J--lIru-l

80-1

?5-l

to-l

ru-1

g eo_i

NL:0m/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MS21658

@I't'v

%

1001

*lnol^-l'-l80-l_-l, t-ltol*l""-l*l50-l

4s-]I

oo-]

*lro-l

Time (min)(rEq

C:XcalibuA...\Negativelon\21659 OTCLAI Cl3 ff7 02116107 11:14:58

NL: 6.45E4rrlz=272.i273.5F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21659

lool t itru'l I.t I

4.33E3n!z- 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21 659

oo6

.Eo

10(

Y'

9(

8!

7(

5l

4(

5(

: 8.89E5fi'lz= 2A2.a-28/..1F: - cESI SRM [email protected] [282.7U2U.251 MS2t659

't0

0

Time lminl


NL: 2.28E5nvz= 299.5-300.5 F: - cESI SRM ms23,[email protected] [299.50-300.50,325.50-326.501 MS21659

NL: 1.82E4r/z= 325.+326.5 F: - qESI SRM [email protected] [299.50-300.50,325.50-326.501 MS21659

@a-14,u

NL:6.35E4r/z=311.5-312.5F:.cESI SRM ms2356.00@15,00 [311,50-312.501 MS21659

'l'ime (min)

C:U<'caliUurt...tNegative lon\21660 OToLololS TrB 02116107 11.'25:5'l

NL: O

tt{z= 272.5-273.5 F: - cESI SRM [email protected] [246.fi-247.50.272.s0-273.501 MS21660


,oo-l

ru-1

*-lru-l

80-l

'lto-l

*-lI 60_l

NL: 6.81 E3rvz= 2995300.5 F: - cESI SRM [email protected] I299.50-300.50.325.50-326.50t MSz toou

6.1 8E3

m/z= 325.5-326.5 F: . cESI SRM [email protected],325.50-326.501 MS21660

@N

oo

€o

66

@}\^\/

v.ocEz10(

9:

8(

7(

filz=282.*2U.3F.-cESI SRM [email protected] I282.7*2U.251 MS

c{u qv

r/z= 311 .5-3'12.5 F: - cESI SRM [email protected] I311 .50-3'12.501 MS21550

4Ar\l,,

C:XcalibuA...\Negative lon\21661 OToLol ol? JjE 0?/16107 11:36:47

NL:3.82E3rilz=272.5-273.5F: -cESI SRM ms2291.20@'t 5.00 [246.fi-247.50,272.50-273.501 MS2'1661

rtlz=246.5-247.5 F: - cESI SRM [email protected] [246.50-247.fi,272.50-273.501 MS21661

ntlz=282.d-284.3 F: - cESI SRM [email protected] I282.75-284251 MS21 661

li, q

@Atl

I

o

.goE

Time (min)


NL:0nvz= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.501 MS21661

3.61E3t/z= 325.&326.5 F: - cESI SRM [email protected] [299.50-300.50,325.s0.326.501 MS21661

. e totr?n/z= 31'1.5-312.5 F: . cESI SRM [email protected] [3't1.50-312.501 MS21661

Time (min)

C:XcalibuA...\Negative lon\21662 OToLO/ A B TDtE 02116107 1 1:47:36

1.01

u-63 NL:8.01E3rrlz= 272.+273.5F: - cESI SRM [email protected] [246.50-247.50,272.s0-273.501 MS21662

nlz= 246.5-247.5 F: - cESI SRM [email protected],272.50-273.501 MSzt00z

1001

ru-l

rol--l

--l*lru-l

to-]

tt-]I 60-l-l

@to

5

o

!o

5.1 0E5filz= 282.8-2U.3F: - cESI SRM [email protected] I282.75-2w.2sl MSz tooz

c{* aV,/ rn t:.Time (min)

Spot LOD, 1uL Q49

NL: 2.98E4-m/z= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.s01 MS2'1662

rn/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSztooz

4.02E3

1.56E5rfl/z= 31 1.5-312.5 F: - cESI SRM [email protected] [311.50-312.501 MS

Time (min)

C:U(calibuA...\Negative lon\21663 07o 20lo tZ TOg BLANK (neg blood, Dl H2O ext.)

@Moc

to

o

@qv

0?/16107 11:58:29

NL: 0

nlz= 272.5-273.5 F: - cESI SRM [email protected] [246.fi-247.50,272.50-273.501 MS21663

NL:5.02E3r/z= 299.5-300.5 F: - cESI SRM [email protected] [zw,cu-Juu.il,325.50-326.501 MS21663

rrvz= 325.5326.5 F: - cESI SRM [email protected] [299.5G300.50.325.s0-326.501 MS21663

n/z= 31 1 .$.312.5 F: . cESI SRM [email protected] [311.s0-312.s01 MS21 663

trlz=246.5-247 ,5 F: - cESI SRM [email protected] [246.fi-247.50,272.50-273.s01 MS21 663

10(

ta

7C

oa

OL

55

c!

45

40

J!

30

:9.09E-l

Time (min) Time (min)

BLANK (neg blood, Dl H2O ext.)C:Wcalibur\...\Negative lon\21664 OToLtJ I olj jDB 0A17107 12:09:21

nlz=282,8-2U.3F:- cESI SRM ms2303.20@ rs.00 [282.75-284.251 MS2166/.

iio vv

1001

*-1

*-lru-l

ro-l

ru-]

70-..1

"]I 60-l

@Nil

1001

oaJ

;;lI*-]

uo-l

--lro-J

'1ro-]

*luo-l

ou-]

oo-]

*t'o-]

NL:7.62E3rnlz=272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MS216&1

r,lr-248-*247.5 Fi - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MS2't664

C:U(calibuA...\Negative lon\21665 O TOLo I a lj -TDB

41

10

5

0

0?/17107 12:20:10

).01U.UJ NL:1.96E4

fflz= 272 .5-273 .5 F : - cESI SRM [email protected] [246.50-247.50,272.5G273.s01 MS21665

ttlz=246.5-247.5 Fi - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21665

ffi.lz=282&2U.3 F: - cESI SRM ms2303,20@ r5,00 [282.7s-2U.251 MS21 665

1 00-i

--l"n-l

,::

;.1--lru-]

:f, "--l

ro1

ss-j

I 60--l oP

E

;

Time (min)

Spot LOD,2 uL Q49

NL: 6.38E4ffVz= 299.5-300.5 F: - cESI SRM msz344,[email protected] I299.50-300.50,325.50-326.501 MS21 665

6.1 8E3m/2= 325.$326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MS21665

7.c/'E4rnlz= 311.t312.5 F: - cESI SRM [email protected] I31'1.50-3'12.501 MS21665

6,,P

Time (min)

C:D(cafiburl...\Negative lonl21666 OToLolotS J^op 0?J17107 12:31:06 BLANK (neg blood, Dl H2O ext.)

J./O NL:4.74E3.n'lz=272,+273.5F: . cESI SRM [email protected] [246.fi-247.50,272.50-273.501 MS21666

n!z=246.1247.5F:- cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21666

ftlz=282.8-2$3F: - cESI SRM [email protected] [282.7$284.251 MS21666

NL:8.98E3rn/z= 299.$300.5 F: - cESI SRM [email protected] {299.50.300.50.s25.50-326.501 MS21666

m/z= 325.5-326.5 F; - cESI SRM [email protected] [299.50-300.50,325.5G.326.501 MSztooo

rvz= 31 1.5-312.5 F: - cESI SRM [email protected] I311.50-312.s01 MS2'1666

, t*l9$"]

'.lI

@ftJ

oP

E

to

66@

^P


fnstrument Method: EDTA_Neg_Swabs. meth

LCe fnstrument Method

Creator: AdministratorLasr modified: z/t6/07 by AdministratorMS Run Time (min) : 10.00

Divert Valve: Dot used during run

MS Detector Settinss:

Segrment 1 fnformation

Duration (min) : 10.00Number of Scan Events: 4Tune Method:

Scan Event De

EDTA_NEG

tails:(291, .2 ) - >oS (246 . s-247 . s

CE L5 . 0? IsoW i_. 0

(303 . 2) ->os (282. B-294.3)CE 15.0? fsoW l_.0

G+e .2) ->oS (299 .5-300. 5CE l-5. 0t f soW 1. 0

(3s5.0) ->oS (srr. s-312. s)CE 15. 0t IsoW l-. 0

l_

2

4

NegMS/MS

NegMS/Ms

NegMS/MS

NegMS/MS

272.s-273 .5)

32s.s-326.s)

Friday, February 15, 2OO7 05i :0 7 z j,4

{a 4+t-Page 1 of 2

CloLc:t e 17

oz lr,o I z.o-?/ tqc\

Instrument Method: EDTA_Neg_Swabs . meth

Thiaafnr narematare.

Syringe draw rate (pI/sec)Tn'i onn i nn rrn l rrma / rr 'l \ ' E\ F_ / ' v

Drrmn cal- f i nae .

Solvent A:80: 20 ACN:WaterSolvent B:BQn l rrant t"'1'

Solvent D:DMin nroccrrra /PqT\ . n

\!v+, . v

Mav nroccrrra /PqT \ . qnnn\!vf /.vvvv

l'hart nrrfnrrf . DroqqrrraCh: r1- nrrf nrri . Nn11116f

f]r:di ont hrnftitm r

Time (nin) Flow (mI,/min)0. 003. 00

0.300.30


Switch L:No changeSwitch 2:No changeSwitch 3:No changeSwitch 4:No change

T ime (mi n ) Event0. 00 Switchl

Waters 2690 LC System

+ 0.038 NH40H

A(r) B(r) c(E) D(*)100. 0 0. 0 0.0 0. 0100.0 0.0 0.0 0.0

Action ParameterNo change

CurveLinearLi-near

-5-6

2007 05:07:I4

5u q'/uf r ar1\

Page 2 of 2(r'/ oL<>l c-.\3

ozfrrofLaa--/D

Friday, February 16,

:

Sample Name:

Conment:

Sequenc e---07 020 1 0 1 3-Neg.sld [Open]

(neg blood, Dl H2O exl

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path

Unknown 21634 C:U(cal ibu r\Data\B rewer\07020 1 0 1 3\N eg ative lon

lnst Method Proc Method CalFile Position InjVol Level Sample Wt

C :Xcal i bu r\methods\E DTA-Neg-Swabs 1I 5.0 1.000

Sample Vol ISTD AMt Dil Factor

0.u00 0.000 1.000

Sample Name:

Comment:

Control (-EDTA blood swab ext.)

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Samole lD Path

Unknown 21635 02 C :U(calibur\Data\B rewer\07020 1 0 1 3\Negative I or


:Xcalibur\methods\EDTA z 5.0 0.000

Samole Vol ISTD AMt Dil Factor

0.000 0.000 1.000

fr aqcb"q

page 1

Dl oL o\ ol3a tl I ulto"1

ToP

Sarnple Name:

Cornment:

Sequence---07 0201 0 1 3_Neg. sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21636 01 C:\)(calibuAData\BreweA070201 0 1 3\Negative lon

Inst Method Proc Method Cal File Position InjVol Level Sample Wt

C:Xcalibur\methods\EDTA Neo Swabs 1 5.0 0.000

Sample Vol ISTD Amt Dil Factor

0.000 0.000 1.000

i**************t****t****************l*****t**+**t*********************************t********i*********

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:

mple Type File Name Sample lD Path

Unknown 21637 01 C:Xcalibur\Data\BreweA07020 1 0 1 3\Negative lon

Inst Method Proc Method Cal File Position InjVol Level Sample wtC : Xcal i bu r\methods\EDTA_N eg_Swabs 1 5.0 0.000

Sample Vol ISTD Amt DilFactor

0.000 0.000 1.000

****ii*********************************************

/tu 4qc,(;. i\

page2

ALrt''Q'la?-o lc13ezfralt""l

-i-r.,p

Sample Name:

Comment:

Sequence---07 0201 0 1 3_Neg.sld [Open]

eltract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21638 03 :U(ca|i bu AData\Brewer\O7020 1 0 1 3\Negative I on

Inst Method Proc Method CalFile Position InjVol Level lSample WtC:\Xcalibur\methods\EDTA Neo Swabs 3 5.0 0.000


0.000 U.UOO 1.000

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Patn

Unknown 21639 01 C :\Xca I i bur\Data\Brewer\07 020 1 013\Negative lor

Inst Method Proc Method Cal File Position InjVol ilevel SamFte WtC:Xcalibur\methods\EDTA Neq Swabs 1 5.0 I 10.000


0.000 0.000 1.000

E q,/orr" )

c,Tolotol3or.l ru I u.:.1

_J_pp

paqe 3

Sample Name:

Comment: Study:

Client:



Laboratory:

Company:

Phone:


Unknown 21640 01 C :U(calibuAData\Brewer\07020 1 0 1 3\N egative lon

lnst Method Proc Method CalFile Position InjVol Level Samole Wt

C :Xcalibur\methods\E DTA-Neg-Swabs 1 5.0 0.000


0.000 0.000 1.000

*********************i*tt***********t****i***********

Sample Name:

Comment:

Q46 extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21641 04 C: U(cali buAData\B rewer\07020 1 0 1 3\Negative I or

lnst Method Proc Method CalFile Position InjVol Level lSample

C : U(cal ibu r\methods\EDTA-Neg-Swabs 4 5.0 0.000


0.000 0.000 1.000

t************i**********************tt

fr qu,( aoz)

nan.a A

O-lol.a\ o\3or-frc lt-oo'l

Ttf

Sample Name:

Comment:

Seq uenc e---07 020 1 0 1 3_Neg. sld [Open]

(neg blood, ext.)

Study:

Client:

Laboratory:

Company:

Phone:


unKnown 21642 01 C :U(calibuAData\Brewer\O7020 1 0 1 3\Negative I or.

Inst Method Proc Method Cal File Position InjVol Level Samole Wt

C:Xcalibur\methods\EDTA Neo Swabs 5.0 0.000


u.000 0.000 1.000

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21643 01 :Xcalibur\Data\Brewer\07020 1 0 1 3\Negative lon

lnst Method Proc Method Cal File Position InjVol Level Sample Wt

C :Xcal ib u r\methods\EDTA_N eg_Swabs 1 5.0 r0.000


0.000 0.000 1.000

{* ++c,(a"4)

oaqe 5

01 oLolr:13or-lrr"lr-"'1

-fl,p

Sample Name:

Comment:

Sequenc e---07 0201 01 3_Neg.sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:

m File Name Sample lD Path

Unknown 121646I

01 G :Xcalibu r\Data\Brewer\07 0201 013\Negative I on


C : U(ca I ibu r\method s\EDTA_N eg_Swabs 5.0 0.000

Sample Vol STD Amt DilFactor

0.000 0.000 1.000

************t****l

Sample Name:

Comment:

Q47 extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21647 06 C :\Xcali bu r\Data\Brewer\07 0201 01 3\Negative I on

lnst Method Proc Method Cal File Position InjVol Level lSamole Wt

C : U(ca I ibu r\methods\E DTA-N eg-Swabs 6 5.0 r0,000


0.000 0.000 1.000

************* t***t*************************

n ,/!G( tr,t)

page 7

Cl o'yo\ olJ

or I ic f r-o. '7

TDP

Sample Name:

Comment:

Sequence---070201 0 1 3_Neg.sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21648 01 C:U(calibuAData\Brewer\07020 1 0 1 3\Neqative lon

lnst Method Proc Method Cal File Position InjVol Level Sampre wtC :Xcali bu r\method s\EDTA_Neg_Swabs 1 5.0 0.000


0.000 0.000 1.000

t*t******************s**********tt**tr********s*r***********************

Sample Name:

Comment:

(neg blood, ext.

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21649 01 C :\Xcalibu r\Data\Brewer\07 0201 01 3\Neg ative I on


C : Xcali bur\method s\EDTA_N eg-Swabs I b.L)10.000


0.000 0.000 1.000

f, '-/4 G(t"4page I

o-lot-a 1o 1 3

"v!t elvolTvp

Sequence--07020 1 0 1 3_Neg.sld [Open]

Sample Name:

Comment:

K4 extract

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type Frle Name Sample lD Path

Unknown 21650 07 C :U(calibu AData\Brewer\07020 1 0 1 3\Neoative lo n

lnst Method Proc Method CalFile Position lnjVol Level Samole Wt

C:U(calibur\methods\EDTA Neo Swabs 7 5.0 0.000


0.000 0.000 1.000

Sample Name:l BLANK (neg DI

Comment:

ext.)

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21651 01 C :Xcal ibur\Data\Brewer\07 0201 0 1 3\Neoative I on

lnst Method Proc Method CalFile Position lnjVol Level lSample

Wt


Vol ISTD Amt Dil Factor

0.000 0.000 1.000

{n'/+(-(^" r)

oaoe 9

a1cl/ol o l?crlrcfi-.'1

-5bp

Sample Name:

Comment:

Sequence---07020 1 0 1 3_Neg.sld [Open]


Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21652 01 C:XcalibuAData\Brewer\070201 0 1 3\Negative lon

lnst Method Proc Method Cal File Position lnjVol Level Sample Wt

C :U(cal i bu r\methods\EDTA_N eg_Swabs 1 5.0 0.000


0.000 0.000 1.000

l********t*****************t*****t*****tt*f*********************i***************************************t*t****r**ti***

Sample Name:

Comment:

Q48 extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21653 08 C:Xcalibur\Data\Brewer\070201 0 1 3\Negative lon

lnst Method Proc Method Cal File Position lnjVol Level lSamole Wt

C :XcalibuAmethods\EDTA_Neg_Swabs 8 5.010.000

Samole Vol ISTD Amt DilFactor

0.000 0.000 1.000

{ q(L,(t.D

oaqe 10

0"1 eLol alT

oultd f r'.'"1

1vP

Sample Name:

Comment:

Seq uenc e---07 020 1 0 1 3_Neg. sld [Open]

(neg ext.)

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21654 01 C:XcalibuAData\Brewer\070201 01 3\Negative ton

lnst Method Proc Method Cal File Fosition InjVol Level Sample WtC: U(cal ibur\methods\E DTA_Neg_Swabs 5.0 0.000


0.000 0.000 1.000

Sample Name: K (neg blood, Dl H2O ext.)

Comment: Study:

Client:

Laboratory:

Company:

Phone:

mple Type File Name Sample lD Path

Unknown 21655 01 C : U(cali bu r\Data\Brewer\07 0201 01 3\Neg ative I or


U.UUO 0.000 1.000

{, q+.(ao'j)

naoe 1 1

cloLot o t3

czlt' lto"1-pP

Sample Name:

Comment:


Pos. ext.

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21656 09 C :U(calibuAData\Brewer\07 0201 013\Negative lon

Inst Method Proc Method CalFile Position InjVol Level Sample WtC : Xcalibu r\methods\EDTA-Neg_Swabs 9 b.0 U.OUO

Sample Vol STD Amt Dil Factor

0.000 0.000 1.000

Sample Name

Comment:

BLANK (neg blood, ext.)

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21657 01 C:U(calibur\Data\Brewer\070201 0 1 3\Neqative lon

Inst Method Proc Method CalFile Position InjVol Sample WtC:Xcalibur\methods\EDTA Neo Swabs I 5.U t0.000


0.000 0.000 1.000

******l*******************ff*************************#******t*************************

{o uo,(;t)

oaoe 12

AloLcl al?olltclr".1

5up

Sequenc e--07 0201 0 1 3_Neg. std [Open]

Sample Name: (neg blood, Dl H2O ext.)Comment: Study:

Client

Laboratory:

Company:

Phone:

Sample Vol ISTD Amt DilFactor0.000 0.000 1.000

Sample Name:

Comment:

****t*****tt*******trt******t*******************

Pos. Cont. B (Q49 ext.

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21659 10 ;:xcattbur\Data\Brewer\O70201 0 1 3\NEetivelon

Inst Method Proc Method Cal File Position InjVol Level Samtte Wt: U(cal i bu r\method s\E DTA_Neg_Swa6! 10 5.0 U.


0.000 0.000 1.000

*******************************************************t******

{n(

4(AJt t;13

o-?oLol r"" l3

aLlrclb-1.TVF

Sample Name:

Comrnent:


BLANK (neg blood, Dl H2O ext.

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21660 01 C :Xcali bur\Data\Brewer\07020 1 0 1 3\Negative I on

Inst Method Proc Method Cal File Position InjVol Level Sample WtC:\Xcalibur\methods\EDTA Neo Swabs 1 5.0 U.OUO


0.000 0.000 1.000

Sample Name:

Comment:

BLANK (neg elit.

Study:

Client:

Laboratory:

Company:

Phone:

sampre rype Frle Name Sample lD Path

Unknown 21661 01 C:U(cali bu r\Data\BreweA07020 1 0 1 3\N eg ative I on

lnst Method Proc Method CalFile Position InjVol Level lSamole Wt

C:Xcalibur\methods\EDTA Neq Swabs 1 5.0 0.000

Sample Vol ISTD Amt lDil Factor

0.000 0.000 1.000

{* ou,1;'a)

oaoe 14

^ A,\,V, V'

0?o1-o\rc't3oLlttluo.'7

'lvp

Sequenc e--07 020 1 O 1 3_Neg. std [Open]

Study:

Client:

Laboratory:

Company:

Phone:


0.000 0.000 1.000

t*t*************************t*f***************************t***t********t*****************************#*****************************r******

Sample Name: neg blood, Dl H2O ext.)

Comment: Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21663 101

C : Xca I i b u r\Data\B rewer\@


0.000 0.000 1.000

***************i*************t**********i***********************t**************t**********i***********************************f***************

f, 4va'(a,z)

6loL ti lo l3a:-J (c lr-,.r

-Ttti'

Seq uenc e---07 020 1 O 1 3_Neg. std [Open]

Sample Name: K (neg blood, Dl H2O extJComment: Study:

Client:

Laboratory:

Company:

Phone:

sample vol ISTD Amt DilFactor0.000 u.u00 1.000

**************************************t*****i**t**************i***t*******************t**t********r*****************************************

Sample Name:

Comment:

Spot LOD, 2 uL

Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21665 12 rv : \AcatrDu r\uaE\tsrewer\O/020 1 0 1 3\Negative I on

Level lSample Wt

Sample ISTD Amt Dil Factor

0.000 U.UOO l.UUO

*****************************************+***********************

a4 VV L,." .\

( r_'+ )nana'14

61aLol o l3alflofr--o?

Tlr0

Seq uenc e--070201 01 3_Neg. std [Open]

Sample Name:1- | - -"-'' I

uomment: Study:

Client:

Laboratory:

Company:

Phone:


Unknown 21666 31 C:U(calibuAData\Brewer\0702O1 0 1 3v\legm lon

Inst Method Proc Method lCal Fite Position InjVol Level Sample WtL; : \Xcal ibu r\methods\E DTA_Neg_Swabs 1 5.0 u.000

Samole Vol ISTD Amt Dil Factor

0.000 0.000 1.000

*****************i*****t**********t****************************************************t**********t************************r****************t

g'J tt>ct tt 19

crr- \tLlr-"-'7-Tt9

t(a

nana 17

44 c-

,)

' Vial List--C:Xcalibur\methods\brewer\070201013\070201013_Neg.std

Position Sample Type Level Sample lD Sample Name1

3

Unknown 1 BLANK (neg blood, Dt H2O ext.)Unknown 02 Neg. Control (-EDTA blood swab ext.)Unknown 03 t(2 extract


c Unknown 05 K3 extract

o Unknown 06 Q47 extract

7 Unknown 07 K4 extract


9 Unknown 09 Pos. Cont. A (MAL EDTA ext.)10 Unknown 10 Pos. Cont. B (Q49 ext.)11 Unknown 11 SpotLOD, luLQ4g12 Unknown 12 Spot LOD, 2 uL Q49

a;'l "L'o\':\7"Z f

tr"lz,,*J.TDS

z* 44C/-\

/ ,-tr 4" )'_/

SOPs

5, q'l'-'(t,r)

-4r

F

FBI LaboratoryChemisry Unit

Toxicolory SubunitTox 4 I 3-0.doc

Issue Date: 0Zll5/07Revision: 0Page I of9

Analysis of EDTA in Dried Bloodstains

1 Introduction

The collection of blood at crime scenes and for legal proceedings is a common practice that maybe used to inculpate or exculpate individuals susp;ct;d of being involved in the-crime.occasionally, there are allegations that blood evidence collecteO f.or crime scenes was ,,planted',.This issue may be resolved by the determination of exogenous components in the bloodstains (e.g.preservatives) that should not be present in authentic crime scene evidence.

Ethylenediaminetetraacetic acid (EDTA) is an anti-coagulant and enzyme inhibitor that iscommonly used in blood specimen collection tubes. Blood specimen collection tubes containingEDTA have lavender-colored tops and are the most common collection tube used to collectreference specimens for DNA testing. Therefore, most allegations of blood evidence ,,planting,,focus on EDTA-preserved blood samples.

EDTA-preserved blood tubes use either the disodium, dipotassium, or tripotassium salt forms ofEDTA. The concentration of EDTA in its free acid form in a drawn blood tube is fypically1000-2000 mg[-, depending on the volume of blood and the capaciry of the tube. At thisconcentration, the free acid and salt forms of EDTA are soluble in the blood. EDTA readily formswater-soluble chelates with nearly all heavy metals, so aqueous extractions of dried blooditainsshould isolate EDTA.

2 Scope

This procedure allows for the screening and confirmation of EDTA in suspected blood stains.

3 Principle

This method takes advantage of the water solubilify of EDTA and EDTA-complexes. A driedbloodstain is first extracted with deionized water and then subjected to ultrafiltiation. Followingultrafiltration, the filtrate is analyzed by liquid chromatography/mass spectrometry/massspectrometry (LCA4SA4S) in both the positive and negative electrospray ionization (ESI) modes.

4 Specimens

This procedure can be used for assaying bloodstains from a cotton swab or other cotton-basedmatrices.

This is an uncontrolled copy of a controlled document.

n qlb/:,<\

b.

d.

e.

f.

FBI LaboratoryChemistry Unit

foxicology Subunit

,,,,.;lJ,oji;lro,;;

ff;J;'r,3

5 E q uipmen t/lVlaterials/Reagents

Guidance for the preparation of reagents may be found inthe preparation of chemical Reagentsstandard operating procedure flox iO:).

a' Liquid chromatograph/mass spectrometer equipped with a Hamilton pRp-l polymericcolumn (2.I mm x 150 mm x 5pm) or equivalint

Laboratory scissors

Millipore Amicon ultra-4 10,000 Molecular weight cutoff centrifugal Filter Device

Wheaton (or similar) pipette - 200 pL

Centrifuge

EDTA-preserved whole blood

EDTA-free whole blood

Deionized water

Acetonitrile (HPLC grade)

Ammonium Hydroxide (HPLC grade)

Deionized water (9s%) / Acetonitrire (s%) / Ammonium Hydroxid e (0.06%)_ MobilePhase for Positive Electrospray Ionization

Acetonirrile (80%) / Deionized water (20%) / Ammonium Hydroxid e (0.03%)_ MobirePhase for Negative Electrospray Ionization

Common laboratory supplies such as glassware, pasteur pipettes, etc.

6 Standards and Controls

EDTA LCA4S/MS(ESI) performance Mix_ 100 pglml-:Accurately weigh r2.7 mgof the disodium saltofE-DTA (reagent grade, Ardrich) anddilute with deionized water to a final volume of 100 rnr. btoie at room temperature in aclear glass container. Stable for at least 6 months.


{u uut/\(,) /,;\

b.

FBI LabontoryChemisrry Unit

Toxicology SubunitTox 413-0.doc

Issue Date:.02l15/07

page 3 of 9

dr2-EDTA Working Internal Standard Solution _ 500 pglml:Accurately weigh 5 mg of the free acid of drz-EDTA i.;d";;grade, cambridge IsotopeLaboratories) and dilute with deionized water to a finar vJlu*Jor l0 mL. store frozen ina brown glass container. Stable for at least 6 months.

Negative Bloodstain Control:Add 50 pL of EDTA-free whore brood to a cotton-tip appricator. Dry for at least 30minutes at room temperature before use. Store at room temperature in a glass test tube orpaper envelope. Stable for at least 2 yeus.

Positive Bloodstain Control :

Add 50 pL of EDTA-preserved whole blood to a cotton-tip applicator. Dry for at least 30minutes at room temperature before use. Store at room t..p.iutur. in a glass test tube orpaper envelope. Stable for at least 2 years.

d.

7 Calibration

This procedure has not been validated for quantitative analysis.

8 Sampling

Not applicable.

9 Procedure

a.

b.

carefully cut the tip from a cotton swab (negative control, positive control, or questionedswab) using clean laboratory scissors.

Place the cotton swab tip into a separately labeled molecular weight cutoff filter device.

Add 200 pL of the drz-EDTAWorking Internal standard Solution directly to each cottonswab tip in the molecular weight cutoff filter device. Allow to sit at room temperature for45 minutes.

centrifuge the molecular weight cutoff firter device for l0 minutes atz500RpM.

copy of a controlled document.

fu uu,/at,r1

d.

This is an uncontrolled

:i:*tHr"#'*''r'i:%:li:::

Issue Date: 02/15/07

ff;:l?3e' Transfer the filtrate to an autosampler vial and inject 5 pL into the LClIr4S/lr4S system thatis in negative ion mode and monitor for both the free acid of EDTA and the EDTA-iron

complex.r SuTll:l that screen positive are confirm.o Ly in;..tion of 5 pL of the filtrateinto the LClIr'IS/l\4S system in the positive ion mode, in wtrich the free acid of EDTA canDe conllrTned.

l0 Instrumental Conditions

10.1 Liquid Chromatograph parameters

10.1.1 Positive Electrospray Ionization Mode

Mobile Phase Composition: Deionized Water (95%) / Acetonitrile (5%) / Ammonium Hydroxide(0.46%)

Column Parameters: Hamilton PRP-I (2.I mm x 150 mm x 5pm) at ambient temperature

Isocratic Flow Rate: 0.3 ml/minute

10.1.2 Negative Electrospray lonization Mode

Mobile Phase composition: Acetonitrile (80%) / Deionized water (20%) / Ammonium Hydroxide(0.03%)

Column Parameters: Hamilton PRP-l (2.1 mm x 150 mm x 5pm) at ambient temperature

Isocratic Flow Rate: 0.3 mllminute

10.2 Mass Spectrometer Parameters

10,2.1 Positive Electrospray Ionization Mode

Spray Voltage: 4.5 kV

Capillary Temperatur e: 230" C

Capillary Voltage: +30V

Collision Induced Dissociation: 100%

' See note on carryover in the Limitations section of this procedure (Section l4).

This is an uncontroiled copy of a controiled document.

L-\a Y'r \r,\/;al\



Issue Date: 02/15107

Revision: 0Page 5 of9

MSA4' Mode: orog:*::f m/z 293.0(EDTA Free Acid)) (m/z 125.0- 3 ls.0);Collision Energy = 15.0%62

Acquisition Time: l0 minutes

10.2.2 Negative Electrospray Ionization Mode

Spray Voltage: 4.5 kV

Capillary Temperatur e: 230" C

Capillary Voltage: -10V

Collision Induced Dissociation: 0% (Offl

SRM Mode: All Collision Energies Set to l5%

Segment I (EDTA Free Acid): m/z 291.2 ) (m/z 246.5-247.5; m/z 272.5-273.5)

Segment 2 (dr2-EDTA Free Acid): m/z 303.2 ) (m/zzg2,g-2s4.3)

Segment 3 (EDTA Iron Complex): m/z 344.2 ) (m/2299.5-300.5;m/z 325.5-236.5)

Segment 4 (d'2-EDTA Iron complex): m/z 356.0 ) (m/z3lr.5-312.5)

Acquisition Time: 10 minutes

11 Decision Criteria

11.1 Performance Mix Suitability

Proper calibration and sensitivity of the LCII\4S/MS (ESI) are demonstrated each day samples areanalyzed. The EDTA LCll\4SA4S (ESI) Performance Mix effectively evaluates rvrr* suitability.Proper mass assignments' elution times, and signal-to-noise responses can be assessed byanalyzing 5 pL of the Performance Mix. In all instances, the elution time should be +zyoof theretention time (relative or absolute) obtained from the previous run's injection of the performanceMix' A stacked Gaussian-shaped peak must be pr.r.ni for the EDTA Free Acid anallte with asignal-to-noise ratio exceeding 50:l for all extracted ions.

' m/z 160 and247 are monitored for EDTA confirmation.

This is an uncontrolled copy of a controlled document./'> '/ t/ /('{ Ll-v Q"/\/ ,?:r. )


t*''r"i:%::l:::

Issue Darc: 02/lS/07Revision:0Page 6 of9

11.2 Analyte Suitabitify

The following criteria are used as guideline_s in determining the acceptabilify of the data producedin this assay. In general, compound identification should 6e based on a comparison of thechromatography and mass spectrometry for the analyte peak of interest with data from acontemporaneously analyzed reference standard or extracted Positive Control. In most cases, allof the following should be met in order to identi8, EDTA within a bloodstain:

ll.2.l Chromatography

The peak of interest should show good chromatographic fidelity, with reasonable peak shape,width, and resolution. Additionally, the following two criteria should be met:

ll,2.l,l Retention Time

The retention time of the peak should be within +ZYo of the retention time (relative or absolute)obtained from injection of the EDTA LCA4S (ESI) Performance Mix, extracted positive control,or the drz-EDTA internal standard.

11.2.1.2 Signal-to-Noise

To justify the existence of a peak, its signal-to-noise ratio must exceed 3. Further, the baselinesignal for the peak from the sample of interest must be at least l0 fold greater than that for anyobserved peak at a similar retention time in a Negative Control or blanf sample injected just priorto that sample.

11.2.2 Mass Spectrometry

The mass spectral results (whether run in SRM mode or full scan products mode) for the analyteof interest should match that ofthe appropriate reference standard or an extracted positive Controlwithin a reasonable degree of scientific certainty. See the Guidelines for Comparison of Massspectra standard operating procedure (Tox 104) for further guidance.

l2 Calculations

Not applicable.


f- +v t-,

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Issue Date: 02/15/07Revision: 0Page 7 of9

13 Uncertainty of Measurement

Not applicable.

l4 Limitations

a' Limit of Detection (LoD): The LoD for EDTA was determined to be 13 pglml in boththe positive and negative electrospray ionization modes. These detection limits weredetermined by triplicate analysis of serial dilutions of an EDTA solution. The lowestconcentration that reproducibly met the decision criteria listed in Section l l above wasdetermined to be the LOD.

b.

A separate LoD study was conducted to determine the minimum volume ofEDTA-preserved blood that was detectable using this analytical method. Three millilitersof whole blood were placed into a 4-mL lavendei-topped blood collection tube containing7'5 mg of EDTA and thoroughly mixed. The EDTA-prbserved blood was placed on a clean,non-porous surface in triplicate at the following volumes: I pL, 5 pL, and l0 pL.Following a I -hour drying period, the blood stains were swabbed using deion lzed waterand cotton-tipped applicators. Each swab was extracted and analyzedio determine theminimum sized EDTA-preserved blood stain required in order to detect EDTA on the swabusing the decision criteria requirements of Section I l. The I pL drop was readilydetectable using this technique.

Selectivity: Selectivity was determined by extraction and analysis of l0 matrix blanks(swabs dipped into different blood samples with a variety of non-EDTA preservativesadded to them). None of the l0 matrix blanks exhibited peaks of EDTA ihat met thedecision criteria requirements of Section I l. Additionally, d12-EDTA was evaluated forinterferences in the analysis and none was observed.

Matrix Effects: Five extracted matrix blanks were spiked with an equal amount of anEDTA standard at both low and high concentrations. Following analysis of these samples,the results were compared with equal concentrations of neat pOfe to determine theamount of ion suppression caused by the blood matrix. While ion suppression was notnoted in the positive electrospray ionization mode, suppression of 3% ind34olo were notedin the negative electrospray ionization mode at EDTA ioncentrations of 50 pglmLand 500p,g/mL, respectively.

Carryover: It has been reported in the literature that trace amounts of EDTA may beabsorbed in the chromatographic system and released in a subsequent analysis of a sample.This carryover was assessed during validation, but was determined to be minor in nafureappearing mainly after the injection of a high concentration of EDTA. To demonstrate the

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il:lT,3lack of carryover within an analytical run, a minimum of two matrix-matched negativesamples (i.e. whole blood extracts) must be analyzed between case samples.

15 Safety

Take standard precautions for the handling of chemicals and biological materials. Refer to the FBILaboratory Safety Manual for guidance.

16 References

Miller, M.L., Mccord, 8.R., Martz, R., and Budowle, B. "The Analysis of EDTA in DriedBloodstains by Electrospray LC-MS-MS and Ion Chromatography", Journal of AnalyticalToxicologt, Vol. 2 l, 1997, 521 -528.

Sheppard, R.L. and Henion, J. "Determining EDTA in Blood", Analytical Chemistry,Vol. 69,1997,477A-480A.

Preparation of Chemical Reagents (Tox 103); FBI Laboratory Chemistry Unit - ToxicologySubunit SOP Manual.

Guidelinesfor Comparison of Mass Spectra (Tox 104); FBI Laboratory Chemistry Unit -Toxicology Subunit SOP Manual.

FBI Laboratory Chemistry Unit - Instrument Operation and Support Subunit SOp Manual.

FBI Laboratory Safety Manual.


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Performance Monitoring protocol (eA/eC)for the Finnigan LCe LCIMS (ESI)

I Scope

This document addresses the performance monitoring (QA/QC) of the Finnigan LCe LCA{Ssystem consisting of a Finnigan LCQ MS and a waters LC. it ls an analytical instrument used toanalyze a wide variety of evidence and must be maintained in such u *uy as to verify itsreproducibility from analysis to analysis and its reliability in court.

2 Principle

The LCQ system is comprised of a Waters Liquid Chromatograph (LC) and a Finnigan ion trapLCQ Mass Spectrometer (MS). The instrument is configurei with an ApI source th-at is capableof both electrospray (ESI) and atmospheric pressure chemical (APCD ionization. Theinstrument is primarily used in ESI mode. However, this protocol can also be used for ApCIprovided the method of ionization is clearly labeled in the resulting data and documentation.Definitions and guidelines for following this protocol are outlined in the ,,General InsrrumentMaintenance Policy."

E q u i p m en t/UIateria ls/Rea gen ts

Instrumentation - Finnigan LCQ MS, API Source, Waters Alliance 2690/2695 LC,and Data System with XCalibur software (or equivalent)

API Gas - Nitrogen, 9999% (high purity or equivalent)

Ion Trap Gas - Helium,99.99%o (high purity or equivalent,l

Methanol, HPLC grade

Deionized Watero 18 MO Milli-e or equivalent

Acetonitrile, HpLC grade

Acetic Acid, reagent grade


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Ultramark 1621 (Finnigan or equivalent)

Caffeine (Sigma or equivalent)

MRFA (L-methionyl-arginyl-phenylalanyl-alanine acetate) (Finnigan or equivalent)

Ammonium Hydroxide (l.lH4OH), reagent grade

Codeine (Sigma or equivalent)

Brucine (Sigma or equivalent)

Reserpine (Sigma or equivalent)

Volumetric glassware

Infusion syringe - l0 to 500 pL LC syringe (Hamilton or equivalent)


4.1 Testmix

The Testmix is used to assess daily operating performance, mass assignment, and continuedintegrity of the system. To prepare, weigh 5.0 mg caffeine, 1.0 mg cod.in", 1.0 mg brucine, and1.0 mg reserpine into a 100-mL volumetric flask. Bring to the mark with methanol and mix well.Store the solution in the refrigerator. It has a shelf-lifJof three years. This preparation may be

appropriately scaled up.

4.2 Calibration Solution

The calibration solution is used for coarse tuning and calibrating the mass spectrometer over theentire mass range. This procedure only needs to be performed when the instiument has beenmoved, down for a long period of time, undergone i major repair, or wananted based on systemperformance.

The calibration solution is a solution of caffeine, MRFA, and ultramark l62l inacetonitrile:methanol:water containing l% acetic acid. To prepare this solution, follow theprocedure in the LCQ'Getting Started'manual. Store the solution in the refrigerator. It has ashelf-life of three years. This preparation may be appropriately scaled up.


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5 Calibration

The calibration procedure should be performed as needed, when the instrument has been moved,down for a long period of time, undergone a major repair, or warranted based on systemperforrnance.

a. Load a 250 1tL syringe with the calibration solution.

b. Using capillary tubing, connect the infusion syringe to the ESI probe assembly, andplace in the syringe pump.

c. Set the syringe pump to the correct syringe fype and set the pump rate tolQpllminute.

d. Load the tune file "ESI_TL|NE" (or equivalent).

e. Check that instrument is in POSITIVE ION mode and collecting CENTROID data.

f. Set the detector using the parameters listed in the 'Instrumental Conditions'section ofthis protocol.

g. Turn on the syringe pump and verif, that the solution is flowing out the ESI needle.

h. Engage the ESI probe and turn on the MS.

i. In Tune Plus, open the Calibrate dialog box, choose the'Automatic'tab and check theindividual tests or'Select All' and then 'Start.'

j. When the calibration is complete, it will display whether or not the calibration wassuccessful.

o Ifthe procedure fails, repeat the calibration.r When the procedure passes, print the report and evaluate the calibration

solution spectrum using the'Decision Criteria' section of this protocol. If theresults are acceptable, print the spectrum of the calibration solution.

k. If all requirements are within specification, prepare the documentation as outlined inthe "General Instrument Maintenance Policy." If any requirements fail, the IOSS


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ff;:1?3Manager will determine the corrective action to be taken.

6 Sampling

Not applicable.

7 Procedures

7.1 Daily Checks

The following steps are to be performed daily. Enter the appropriate information in the eA/eClog for tracking purposes.

Record the remaining disk space on the hard drive. Use Windows Explorer program(WindowsNT) to verifu that the hard disk has at least 100 MB of free disk space-. Donot use if less than 100 MB remain.

Record the line pressure of the building nitrogen supply (ApI gas). The regulatorshould read between 60 and 100 p.s.i. If it cannot maintain thii pressure, contactIOSS. If the nitrogen is supplied by a gas cylinder, record the tank pressure. Changethe tank if less than 100 p.s.i. remaining.

Record the line pressure of the building helium suppry (ion trap gas). The regulatorshould read between 30 and 60 p.s.i. If it cannot maintain this pressure, conracrIoss. If the helium is supplied by a gas cylinder, record the tank pressure. changethe tank if less than 100 p.s.i. remaining.

Check the Ion Gauge to ensure that no significant leaks are present in the system. Donot use if the pressure is higher than I x l0-a torr.

Prepare the instrument for analysis of Testmix. Verifu that the instrument has thecorrect source probe installed (ESI), the correct tune file loaded (esi_tune orequivalent), positive ion mode selected, and centroid data being collected. If acolumn is installed, remove it from that system and replace it wittr the infusioncapillary tube.Perform an analysis of the Testmix prior to the analysis of evidence using parameterslisted in the 'Instrumental Conditions' section of this protocol. Start the ftplC pump.Engage the ESI probe and turn on the MS. Start an acquisition using a filenam! such


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lilii[!as'testmix'(or equivalent). Make three 5 pL injections of the Testmix solutionapproximately l0 seconds apart by using the manual loop injector, and then stop thedata collection. Evaluate the results using the 'Decision Criteria' section of thisprotocol. If the results are acceptabte, print the TIC and spectra for all components inthe Testmix.

g' If all requirements are within specification, prepare the documentation as outlined inthe "General Instrument Maintenance Policy." If any requirements fail, contactIOSS.

7.2 As Needed Checks

b.

Re-cut or replace the sample capillary as needed.

Clean or replace the heated capillary as needed.

8 Instrumental Conditions

Refer to the "General Instrument Maintenance Policy" for procedures on minor deviations.

8.1 Testmix

Liquid ChromatographMobile Phase:Flow Rate:

Column:Inj Volume:Number of Inj:

Mass SpectrometerIonization:Tune File:Scan Mode:Scan Range:

95:5 methanol:water + 0.03% ammonium hydroxide0.2 mllminNone5pL

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8.2 Calibration

Mass SDectrometerIonization:Tune File:Scan Mode:Scan Range:

9 Decision Criteria

9.1 Testmix

ESIesi_tuneFull Scan100-2000 m/z

Verifu the results of the Testmix. The following ions should be observed in the three Testmixinjections:

o Caffeine 195 m/zo Codeine 300 mlzr Brucine 395 mlz. Reserpine 609 mlz

9.2 Calibration

Verify the results of the calibration. The calibration will indicate if the procedure wassuccessful. The individual ions for the calibration solution are:

r Caffeineo MRFAr Ultramark

195 mlz524 mlz1022 mlzll22 m/z1222 mlz1322 mlz1422 m/z1522 mlz1622 mlz1722 m/z1822 mlz1922 mlz

greater than 5Yo

greater than 50%greater than 5Yo

greater than 20o/o

greater than 50Yogreater than 50Yogreater than 80%o

greater than 50%o

greater than 50Togreater than 20%o

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ff;:'il,310 Calculations

Not applicable.

ll Uncertainty of Measurement

Not applicable.

12 Limitations

Only properly trained personnel shall perform duties involved in the operation, maintenance, ortroubleshooting of this instrument.

13 Safefy

Take standard precautions for the handling of all chemicals, reagents, and standards. Refer tothe FBI Laboratory Saf"ty Manual for the proper handling and disposal of all chemicals.Personal protective equipment should be used when handling any chemical and when performingany type of analysis. Many instrument components are held at temperatures of 250oC andhigher. Precautions should be taken to prevent the contact of skin with heated surfaces andareas.

14 References

Manufacturer's Instrument Manuals for the specific models and accessories used.

"General Instrument Maintenance Policy" (Inst 001) Instrument Operation and Support SubunitSOP Manual.

"Liquid Chromatograph General Maintenance Protocol" (Inst 003) Instrument Operation andSupport Subunit SOP Manual.

"Mass Spectrometer General Maintenance Protocol" (Inst 004) Instrument Operation andSupport Subunit SOP Manual.

FBI Laboratory Safety ManuaL


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Preparation of Chemical Reagents

I Scope

This procedure provides instructions for the preparation and storage of all reagents used in thevarious standard operating procedures of the Chemistry Unit's Toxicology Su-bunit. Thisdocument does not provide information for materials used directly as obiained from themanufacturer. Neither does it provide instructions for the preparation of calibrators, controls, oranalytical standards. Prepared reagents are listed, in alphabetical order, in section 6, ,,procedure,,and materials needed for preparation of these reagents are listed in section 2,o,Equipment/Materials/Reagents." Refer to the Chemistry (Jnit Procedure for Verification of'Re'agents, Kits,Solvents and Standards (CUQA 9) for guidance in labeling and testing the reliabilirylf reagents.

2 Equipment/lVlaterials/Reagents

a. Electronic balance

b. pH paper in various ranges

Ultrasonicator

vacuum filtration apparatus (l liter size) with 0.5 pm prFE filter membranes

Miscellaneous routine laboratory glassware and supplies

Acetic acid, glacial(17 M) (ACS grade)

Acetonitrile (HPLC grade)

Ammonium acetate (reagent grade)

Ammonium hydroxide, concentrated (15 M) (ACS grade)

Calcium chloride (reagent grade)

Chloramine T (reagent grade)

Chloroform (GC2 grade and HpLC grade)

o-Cresol (reagent grade)

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n. Cupric sulfate pentahydrate (reagent grade, CuSOa.5H2O)

o. Curcumin (reagent grade)

p. Diethyl ether (high purity grade)

q. Dimethylsulfoxide (ACS grade)

r. Diphenylamine (reagent grade)

s. Ethyl acetate (HPLC grade)

t. Ethyl alcohol (200 proof and pharmaceutical grade)

u. Ferric chloride hexahydrate (reagent grade, FeCls.6HzO)

v. Ferric nitrate nonahydrate (reagent grade, Fe(NO3)3,9H2O)

w. Gold(III) chloride hydrochloride trihydrate (reagent grade, HAucl+.3Hzo)

x. Heptafluorobufyric acid (aka HFBA) (reagent grade)

y. Hexamethonium hydroxide solution, 0.1 M (obtained from Fluka Chemical Company)

z. Hexane (UV grade)

aa. Hydrochloric acid, concentrated (12 M) (ACS grade)

bb. Indigo Carmine (reagent grade)

cc. Iodine (reagent grade)

dd. Isopropanol (2-propanol) (HPLC grade)

ee. Magnesium nitrate (high purity grade I)

ff. Mercuric chloride (reagent grade, HgCl2)

eg. Methanol (GC2 grade and HPLC grade)

hh. Methylene Chloride (dichloromethane) (HPLC grade)

ii. Nitric acid, concentrated (16 M) (ACS grade and optima grade)

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jj. Palladium matrix modifier solution (0.1% obtained from High-Purity Standards,Inc.)

kk. PIC reagent (methanesulfonic acid) (reagent grade)

ll' PICB-8 reagent (octanesulfonic acid) (low UV grade obtained from Waters Corp.)

mm. Potassium cyanide (reagent grade)

nn, Potassium ferricyanide (reagent grade)

oo. Potassium hydroxide (reagent grade)

pp. Potassium iodide (reagent grade)

qq. Potassium phosphate, monobasic (ACS grade, KH2pOa)

rr. Pyromellitic acid (reagent grade)

ss. Saponin (reagent grade)

tt. Silver nitrate (reagent grade)

uu. Sodium acetate trihydrate (reagent grade)

vv. Sodium bicarbonate (reagent grade)

ww. Sodium borate (sodium tetraborate decahydrate) (ACS grade, NazB+oz.l0H2o)

xx. Sodium chloride (reagent grade)

W. Sodium dithionite (reagent grade)

zz. Sodium hydroxide (ACS grade)

aaa. Sodium phosphate, dibasic heptahydrate(ACS grade, Na2HpO4.7H2O)

bbb. Sodium phosphate, monobasic monohydrate (ACS grade, NaHzpO+.HzO)

ccc. Sulfuric acid, concentrated (18 M) (ACS grade)

ddd. Tetramethylammonium hydroxide (ACS grade)

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Toluene (HPLC grade)

Triethanolamine (reagent grade)

ggg. Trifluoroacetic acid (98+% purity)

hhh. Water, Deionized (18+MO grade)


Not applicable.

4 Calibration

Not applicable.

5 Sampling

Not applicable.

6 Procedure

Unless specifically noted otherwise, all reagents can be prepared in larger or smaller total volumes,as needed, by appropriate scaling of component volumes and masses. Listed grades or qualities ofchemicals are the minimum acceptable levels. Unless specifically noted otherwise, a higherquality of the same chemical may be substituted.

a. 50 mM Acetic Acid:To a 100-mL graduated cylinder, add 80 mL deionized water and 0.25 mL glacial aceticacid. Mix well and bring to 85 mL with deionized water. Store in glass at roomtemperature. Stable 3 months.

b. 0.1 M Acetic Acid:To a 100-mL graduated cylinder, add 80 mL deionized water and 0.5 mL glacial acetic acid.Mix well and bring to 85 mL with deionized water. Store in glass at room temperature.Stable 3 months.


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Dilute (- 1.5 M) Acetic Acid:Mix 2 mL glacial acetic acid with 20 mL deionized water and shake to combine. Store inglass at room temperature. Stable 3 months.

I : I Acetonitrile:Water:Combine 100-mL HPLC grade acetonitrile with 100 mL deionized water and mix well.Store in glass at room temperature. Stable 6 months.

0.1 M Ammonium Acetate:Add 3.85 g ammonium acetate to a 500-mL volumetric flask containing 300 mL deionizedwater. Mix well to dissolve, and bring to volume with deionized water. Store inrefrigerated in glass. Stable 2 months.

0.24 M Ammonium Hydroxide:Add 1.6 mL concentrated ammonium hydroxide to 50 mL deionized water in a 100-mLgraduated cylinder. Fill to the 100-mL mark with deionized water and mix well. Store inglass at room temperature. Stable I month.

2 M Ammonium Hydroxide:Add l0 mL concentrated ammonium hydroxide to 50 mL deionized water in a 100-mLgraduated cylinder. Fillto the 75-mL mark with deionized water and mix well. Store inglass at room temperafure. Stable I month.

5% (wlv) Calcium Chloride Solution:Dissolve I g calcium chloride in 20 mL deionized water. Store in glass at roomtemperature. Stable I year.

CE (Capillary Electrophoresis) Run Buffer - Anions:To a 1000-mL volumetric flask, add 500 mL deionized water, 612 mgpyromellitic acid,280 mg sodium hydroxide, 238 mg triethanolamine, and 7.5 mL 0.1M hexamethoniumhydroxide solution. Mix wellto dissolve, and bring to volume with deionized water. Storerefrigerated in plastic. Stable I week.

05% (wlv) Chloramine T:To a 100-mL volumetric flask, add 80 mL deionized water and 0.5 g chloramine T. Mixwell to dissolve and bring to volume with deionized water. Store refrigerated in glass.Stable 6 months.

4: I Chloroform:Methanol:Combine 40 mL GC2 grade chloroform with l0 mL GC2 methanol. Mix well. Store inbrown glass at room temperature. Stable I month.

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l% (by volume) o-Cresol:Place I mL o-cresol in a 100-mL volumetric flask and fill to the mark with deionized water.Mix well and allow to stand for at least 24 hours before use. Store refrigerated in brownglass. Stable 6 months.

5% (w:v) Cupric Sulfate Solution:Dissolve 1.56 g cupric sulfate pentahydrate in 20 mL deionized water. Store in slass atroom temperature. Stable I year.

Curcumin Solution (saturated in ethanol):Add curcumin to l0 mL 200 proof ethanol in a test tube with mixing until no more willdissolve. Centrifuge at low speed for 5 min and transfer the supernatant. Store in glass atroom temperature. Stable 1 year.

Cyanmethemoglobin Reagent (Drabkin's Solution):To a 1000-mL volumetric flask containing 500 mL deionized water, add 200 mg potassiumfenicyanide, 50 mg potassium cyanide, and I g sodium bicarbonate. Mix well to dissolveand bring to volume with deionized water. Store refrigerated in brown glass. Stable 4months.

Diphenylamine Reagent (05% w:v in sulfuric acid):Dissolve 0.5 g diphenylamine in 100 mL concentrated sulfuric acid. Store in glass with aPTFE-lined cap at room temperature. Stable I year.

80% (by volume) Ethanol:Measure 80 mL pharmaceutical grade ethanol into a 100-mL volumetric flask. Bring tovolume with deionized water and mix well, Store in glass at room temperature. Stable for6 months.

l:l Ether:Toluene:Combine 50 mL HPLC grade toluene with 50 mL diethyl ether. Mix well. Store in slassat room temperature. Stable I month.

5% (wlv) Ferric Chloride Solution:Dissolve 1.67 g fenic chloride hexahydrate in 20 mL deionized water. Store in slass atroom temperature. Stable I year.

05% (w/v) Gold Chloride Solution:Dissolve 130 mg gold(IID chloride hydrochloride trihydrate in 20 mL deionized water.Store in brown glass at room temperature. Stable I year.


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u. 0.1% (w/v) Heptafluoroburyric Acid:Add 0.5 g HFBA to 400 mL deionized water in a 500-mL volumetric flask and mix well.Bring to volume with deionized water. Store in glass at room temperature. Stable 3months.

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2mM Hydrochloric Acid:In a 100-mL volumetric flask, combine g0 mL deionized water with l6hydrochloric acid and mix well. Bring to volume with deionized water.room temperature. Stable 6 months.

pl concentratedStore in glass at

0.1 M Hydrochloric Acid:To a 100-mL graduated cylinder, add 80 mL deionized water and 0.8 mL concentratedhydrochloric acid. Bring to 96 mL with deionized water and mix well. Store in slass atroom temperature. stable 6 months.

0.96 M Hydrochloric Acid:To a 100-mL volumetric flask, add 80 mL deionized water. Add S mL concentratedhydrochloric acid and mix well. Bring to volume with deionizedwater. Store in glass atroom temperature. Stable 6 months.

I M Hydrochloric Acid:To a 100-mL graduated cylinder, add 80 mL deionized water. Add 8 mL concentratedhydrochloric acid and mix well. Bring to 96 mL with deionized water. Store in glass atroom temperature. Stable 6 months.

6 M Hydrochloric Acid (- 50% v:v):To a 25-mL graduated cylinder containing l0 mL deionized water, add l2 mLconcentrated hydrochloric acid and mix well. Bring to 24 mLwith deionized water. Storein glass at room temperature. Stable 6 months.

0.01% (w/v) Indigo Carmine Reagent:Dissolve l0 mg indigo carmine in 100 mL deionized water. Store in glass at roomtemperature. Stable I year.

Iodine Test Solution:Dissolve 0.4 g iodine and 0.6 g potassium iodide in 20 mL deionized water. Store in qlassat room temperature. Stable 6 months.

LC (Liquid chromatography) Mobile phase - Alkaline#l / cocaine (95:5:0.03methanol :water:ammonia) :

Combine 950 mL HPLC grade methanol and 50 mL deionized water. Mix well andvacuum filter through a 0.5 pm PTFE membrane. Add 0.3 mL concentrated ammonium

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Issue Date: 10/27/2006Revision. 2

page 8 of 15

hydroxide and mix gently. Veriff pH>8. Store in glass at room temperature. Stable Imonth.

LC Mobile Phase - Alkaline#2 (5:95:0.03 methanol:water:ammonia):Combine 25 mL HPLC grade methanoland 475 mL deionized water. Mix well andvacuum filter through a 0.5 pm PTFE membrane. Add 0.15 mL concentrated ammoniumhydroxide and mix gently. Verif, pH>8. Store in glass at room temperature. Stable Imonth.

LC Mobile Phase - Benzodiazepines (60 :40 :0.03 methanol:water:ammonia):Combine 300 mL HPLC grade methanol and 200 mL deionized water. Mix well andvacuum filter through a 0.5 pm PTFE membrane. Add 0.15 mL concentrated ammoniumhydroxide and mix gently. Verifu pH>8. Store in glass at room temperature. Stable Imonth.

LC Mobile Phase - Rodenticide #l (0.1% acetic acid in water):Vacuum filter 500 mL deionized water through a 0.5 pm PTFE membrane. Add 0.5 mLACS grade glacial acetic acid. Store in glass at room temperature. Stable I month.

LC Mobile Phase - Rodenticide #2 (0.1% acetic acid in methanol):Vacuum filter 500 mL Optima grade methanol. Add 0.5 mL ACS grade glacial acetic acid.Vacuum filter through a 0.5 pm PTFE membrane. Store in glass at room temperature.Stable I month.

LC Mobile Phase - Mivacurium #l (acetonitrile):Measure out 1000 mL HPLC grade acetonitrile and vacuum filter through a 0.5 pm pTFEmembrane. Store in glass at room temperature. Stable 2 months.

LC Mobile Phase - Mivacurium#Z (5 mM octanesulfonic acid):Quantitatively transfer the contents of one vial of PICB-8 reagent into a 1000-mLvolumetric flask and bring to the mark with deionized water. Vacuum filter through a 0.5pm PTFE membrane. Store in glass at room temperature. stable I month.

LC Mobile Phase - Mivacurium MSMS (40 : 60 :0.0 I 5 acetonitrile:water:methanesulfonicacid):Combine 200 mL HPLC grade acetonitrile, 300 mL deionized water, and 75 pl pIC reagent.vacuum filter through a 0.5 pm PTFE membrane, and verifu 2<pH<3.5. Store at roomtemperature in brown glass. Stable I month.

LC Mobile Phase - Succinylmonocholine #l (92:8:0.1 water:methanol:pIC reagent):Combine 460 mL deionized water, 40 mL HPLC methanol, and 0.5 mL pIC ..["ni. tuti*well and vacuum filter through a 0.5 pm PTFE membrane. Store ar room remperature inbrown glass. Stable for I month.


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ll. LC Mobile Phase- Succinylmonocholine #z(80:15:4.75:0.25 0.1% HFBA:g.1 Mammonium acetate:acetonihile: isopropanol) r

Combine 400 mL 0.1% heptafluorobutyric acid,75 mL 0.1 M ammonium acetate,23.75mL HPLC grade acetonitrile, and 1.25 mL HPLC grade isopropanol. Mix well andvacuum filter through a 0.5 pm PTFE membrane. Store in glass at room temperature.Stable I month.

mm. l:l Methanol:Dilule Hydrochloric Acid:Combine 2 mL GC'grade methanol with 2 mL I M hydrochloric acid, and mix well. Storein glass at room temperature. To be prepared fresh.

nn. 95:5 Methanol:Water:Combine 95 mL HPLC grade methanol with 5 mL deionized water and mix well. Store inglass at room temperature. Stable 6 months.

l:l Methanol:Water:Combine 50 mL HPLC methanolwith 50 mL deionized water and mix well. Store in elassat room temperature. Stable 6 months.

Nitric Acid, Dilute (33%by volume):Mix 5 mL concentrated nitric acid with 10 mL deionized water and shake to combine.Store in glass at room temperature. Stable I year.

0.2% (by volume) Nitric Acid:To a 1000-mL Nalgene volumetric flask containing 600 mL deionized water, add 2 mLOptima grade concentrated nitric acid. Bring to volume with deionized water and mix well.Store in plastic at room temperature. Stable I year.

Op iates Extraction Solvent (90 : I 0 chloroform : isopropanol) :

Combine 50 mL HPLC grade isopropanol and 450 mL HPLC grade chloroform and mixwell. Store at room temperature in brown glass. Stable I month.

Palladium / Magnesium Nitrate Matrix Modifier for AAS (Atomic AbsorptionSpectroscopy):To a 100-mL Nalgene volumetric flask containing 50 mL deionized water, add l5 mgmagnesium nitrate and25 mL palladium matrix modifier solution. Bring to volume withdeionized water and mix well. Store at room temperature in Nalgene container. Stable 5years.


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tt. I 1.8 M Potassium Hydroxide:To a 100-mLNalgene volumetric flask add 66 g potassium hydroxide and 50 mL deionizedwater. Mix well to dissolve and bring to volume with deionized water. Store at roomtemperature in Nalgene container. Stable I year.

uu. 5% (wlv) Potassium Phosphate Buffer (pH 4.5):To a 100-mL volumetric flask, add 80 mL deionized water. Add 5 g monobasic potassiumphosphate and mix wellto dissolve. Bring to volume with deionized water, and veri$r4.0<pH<5.0. Store refrigerated in glass. Stable I month.

vv. l0% (w/v) Silver Nitrate Solution:Dissolve 2 g silver nitrate in 20 mL deionized water. Store at room temperature in anopaque container. Stable I year.

ww. 0.1 M Sodium Acetate Buffer (pH 7):

To a 250-mL volumetric flask, add 3.4 g sodium acetate trihydrate and 200 mL deionizedwater. Mix well and adjust to 6.5<pH<7.5 by slow addition of I N hydrochloric acid.Bring to volume with deionized water. Store refrigerated in glass. Stable 2 months.

xx. Sodium Acetate Buffer with 5% Methanol:Add 5 mL HPLC grade methanolto a 100-mL volumetric flask and bring to volume with0.1 M sodium acetate buffer (pH 7). Store refrigerated in glass. Stable 2 months.

yy. 1.1 M Sodium Acetate Buffer (pH 5.5):To a 100-mL volumetric flask, add 14.95 g sodium acetate trihydrate, 60 mL deionizedwater, and2.2 mL glacial acetic acid. Mix wellto dissolve, and bring to volume withdeionized water. Verif 5<pH<6. Store refrigerated in glass. Stable 2 months.

zz. 0.1 M Sodium Borate Buffer (pH 9):To a 100-mL volumetric flask add 3.8 g sodium borate and bring to volume with deionizedwater. Sonicate for l5 minutes to assist dissolution, and verifu 8.5<pH<9.5. Storerefrigerated in glass. Stable 3 months.

aaa. Saturated Sodium Chloride Solution (- 35%wlv):To a 500-mL volumetric flask, add 450 mL deionized water and 175 g sodium chloride.Gently heat with continuous stining for at least one hour. Remove the stirbar, fill tovolume with deionized water, and mix by inversion. A small amount of undissolved solidshould remain in the bottom of the flask. Store in glass at room temperature. Stable forone year.


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bbb. 0.287 M Sodium Dithionite Reducing Agent:To a 50-mL volumetric flask, add 40 mL deionized water and 236 gsodium dithionite.Mix well to dissolve and bring to volume with deionizedwater. Store in glass at roomtemperature. Stable I month.

ccc. 0.1 M Sodium Hydroxide:To a 100-mL Nalgene volumetric flask, add 60 mL water and 0.4 g sodium hydroxide. Mixwell to dissolve and bring to volume with deionized water. Store in Nalgene containers atroom temperature. Stable 1 year.

ddd. 5 M (20% w/v) Sodium Hydroxide:To a 100-mL Nalgenb volumetric flask, add 60 mL water and 20 g sodium hydroxide. Mixwell to dissolve and bring to volume with deionized water. Store in Nalgene containers atroom temperature. Stable I year.

eee. 0.1 M Sodium Phosphate Bufler (pH 6.0):To a 500-mL volumetric flask, add 400 mL deionized water, 6.1 g sodium phosphatemonobasic monohydrate, and 1.6 g sodium phosphate dibasic heptahydrate. tvti* well todissolve. Verifr 5.8<pH<6.1, adjusting pH by addition of 0.1 M dibasic sodium phosphate(increases pH) or 0.1 M monobasic sodium phosphate (decreases pH) as necessary. Bringto volume with deionized water. Store refrigerated in glass. Stable I month.

fff. 0.1 M Sodium Phosphate, Dibasic:To a 100-mL volumetric flask, add 2.7 g sodium phosphate dibasic heptahydrate and 80mL deionized water. Mix wellto dissolve and bring to volume with deionized water.Store refrigerated in glass. Stable I month.

goo 0.1 M Sodium Phosphate, Monobasic:To a 100-mL volumetric flask, add 1.4 g sodium phosphate monobasic monohydrate and80 mL deionized water. Mix well to dissolve and bring to volume with deionized warer.Store refrigerated in glass. Stable I month.

SPE (Solid Phase Extraction) Alkaline / Cocaine Elution Solvent (78:20:2 methylenechloride : isopropanol : ammonia) :

Combine 20 mL HPLC grade isopropanolwith 2 mL concentrated ammonium hydroxideand mix well. Add 78 mL HPLC grade methylene chloride and mix well. Store in slass atroom temperature. To be prepared fresh.

SPE Benzodiazepines Elution Solvent (49:l ethyl acetate:ammonia):Combine 49 mL ethylacetate with I mL concentrated ammonium hydroxide and mix well.Store in glass at room temperature. To be prepared fresh.


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jjj. SPE Benzodiazepines Wash Solvent (20% acetonitrile in 0.1 M phosphate buffer):Combine 80 mL 0.1 M phosphate buffer (pH 6) with 20 mL HPLC grade acetonitrile andmix well. Store in glass at room temperature. Stable I month.

kkk. SPE THC Elution Solvent aka Rodenticide Wash Solvent (95:5 hexane:ethyl acetate):Combine 95 mL hexane with 5 mL ethyl acetate and mix well. Store in glass at roomtemperature. Stable 3 months.

ll l. sPE THC-cooH Elution Solvent aka Rodenticide Elution Solvent (75.25:l hexane:ethylacetate:acetic acid):Combine 75 mL hexane with 25 mL ethylStore in glass at room temperature. Stable

mmm.5NSulfuricAcid:To a 100-mL graduated cylinder containing 70 mL deionized water, slowly add 12.5 mLconcentrated sulfuric acid. Mix well and bring to 90 mL with deionized water. Store inglass at room temperature. Stable I year.

nnn. 5% (by volume) Sulfuric Acid:To a 100-mL volumetric flask containing 80 mL deionized water, slowly add 5 mLconcentrated sulfuric acid. Mix well and bring to volume with deionized water. Store inglass at room temperature. Stable I year.

ooo. I M Sulfuric Acid with I .5% (wlv) Saponin:Add 80 mL deionized water and 1.35 g saponin to a 100-mL graduated cylinder and mixwell to dissolve. Slowly add 5 mL concentrated sulfuric acid. Bring to the 90-mL markwith deionized water and mix well. Store in glass at room temperature. Stable I year.

ppp. THC-COOH Extraction Solvent (7:l hexane:ethyl acetate):Combine 70 mL hexane with 10 mL ethyl acetate and mix well. Store in glass at roomtemperature. Stable 3 months.

qqq. TMAH Reagent:Dissolve 0.25 gtetramethylammoniumhydroxide in I mL deionized water. Add 20 mLdimethylsulfoxide and mix well. Store refrigerated in brown glass. Stable I year.

rrr. 0.04% (by volume) Trifluoroacetic Acid (TFA):To a 100-mL volumetric flask, add 90 mL deionized water and 40 pltrifluoroacetic acid,Mix well and bring to volume with deionized water. Store in glass at room temperature.Stable 3 months.

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FBI LaboratoryChemrstry Unit



Revision: 2Page l3 of l5

sss. Trinder'sReagent:Add 400 mg mercuric chloride, 400 mg fenic nitrate nonahydrate , and 0.1 mLconcentrated hydrochloric acid to 5 mL deionized water in a 10-mL volumetric flask. Mixwell to dissolve and bring to volume with deionized water. Store refrigerated in glass.Stable 6 months.


Not applicable.

8 Decision Criteria

Not applicable.

9 Calculations

Not applicable.


Not applicable.

11 Limitations

Not applicable.

12 Safety

Follow standard precautions for the handling of chemicals and biological materials. Refer to theFBI Laboratory Safety Manual for guidance.


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13 References

Shugar, G. J.; Ballinger, J.T. Chemical Technicians' Ready Reference Handbook, 3'd Ed;McGraw-Hill: New York. NY. 1990.

FBI Laboratory Safety Manuol,

Toxicologt Subunit SOP Manual.

Chemistry Unit Procedurefor Verification of Reagents, Kits, Solvents and Standards (CUQA 9);FBI Laboratory Chemistry Unit Quality Assurance Manual.


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Rev. # Issue Date History%

0 l/30/06 New document.

L 6121106 Added new reagent (saturated sodium chroride), and removedseveral (insulin ELISA reagents).

tat27/a6 Added new reagents (mobile phases for rodenticides).

Apnroval ; A//l V nChemistry Unit Chief: ' I/UUW fu#-(*- Date:

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OA Apnroval

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Issuance

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Guidelines for Comparison of Mass Spectra

I Introduction

Many of the analytical procedures used in the Toxicology Subunit rely on mass spectrometry tohelp establish identification of individual chemical entitils within a sample. In oider to ensureconsistency and reproducibility in compound identification, it is desirabie to have guidelines forthe comparison of known and unknown mass spectra.

2 Scope

This document provides guidelines to help determine what constitutes a match between knownand unknown mass spectra. Various critical characteristics of a mass spectrum are defined, andprocedures for using these characteristics to evaluate matching between spectra are laid out. Notethat this document provides guidelines for the matching of miss spectra, and does not directlyaddress compound identification. A good quality masJspectral match will normally be onlytneelement in establishing the identity of an unknown substance. These protocols are intended forapplication to full scan, tandem, and selected ion monitoring (SIM) mass spectra acquired inelectron impact (EI), chemical (CI), electrospray (ESI), and atmospheric piessure chemicalionization (APCI) modes. other mass spectral techniques are beyond the scope of this document.

3 Principle

The spectrum of a given unknown of interest is compared to the known spectrum of a targetanalyte. The unknown spectrum should contain all the significant ions present in the knownspectrum, and should not contain any unexplained significant ions not seen in the known spectrum.The relative intensities (hereafter referred to as "ion ratios") of several selected characteristic ions

should match in both spectra, to within defined tolerances. These guidelines draw heavily ontechnical document 2003IDCR from the World Anti-Doping Agency, the 2003 recommendationsof the American Society for Mass Spectrometry's Measur.r.nts and Standards Committee, andthe2002 National Committee for Clinical Laboratory Standards Approved Guideline for GC/Tr4S(gas chromatography/mass spectrometry) Confirmation of Drugs.

4 Specimens

Not applicable.

5 Equipment/Materials/Reagents


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Not applicable.


Not applicable.

7 Calibration

The calibration of all mass spectrometers should be verified regularly per the appropriateinstrument protocols inthe Instrument Operations and Support Subunit SOP Manual.

8 Sampling

Not applicable.

9 Procedure

Provided below are procedures for defining and determining critical characteristics of a mass

spectrum to be used in establishing whether or not two spectra match. An abbreviated list of the

key points is provided in Appendix L

9.1 Averaging and Background Subtraction of Mass Spectra

In many real-world samples, it may be necessary to correct mass spectra of interest for the

presence of ions resulting from sample background, instrument background, or partially coelutingsample components. The necessary background-subtracted spectrum will usually be generated byaveraging not more than five spectra across the peak of interest and then subtracting the average

of a number of background spectra equalto not more than twice the number of sample spectra. Thebackground spectra may come before and/or after the sample spectra, and should all be selected

from outside the region integrated for determination of ion ratios. This background-subhacted

spectrum will be used to establish the list of significant ions and the base peak for that spectrum.

9.2 Determination of "Significant lons" in a Mass Spectrum

Any ion signal greater than l5% of the most intense ion signal in a background-subtracted mass

spectrum will normally be considered a signiJicant ion. An ion that would otherwise be

considered significant may be excluded if it can be demonstrated that the ion arises from, or issignificantly disturbed by, an uncorrectable chemical interference. Such interferences will


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normally be demonstrated by showing that a reconstructed ion trace for the ion in question is not

coincident with the traces for other ions associated with the component of interest.

9.3 Determination of "Diagnostic Ions" in a Mass Spectrum

Diagnostic ions are those ions in a mass spectrum that are characteristic of the chemicalcompound under investigation. Determination of diagnostic ions depends upon knowledge of the

chemical structure of a component under investigation, and may therefore only be determined

from mass spectra of known standards. The definition of what makes any given ion

"characteristic" of a particular chemical structure is somewhat nebulous, and there does not appear

to be any universally accepted standard in the field. This means that good and consistent judgment

by the examiner is essential. There are, however, recommendations as to what renders some ions

nonspecific and not diagnostic, and an examiner should abide by these practices when eliminatingions from consideration as diagnostic.

Adduct ions will normally be excluded, except that one pseudomolecular adduct ion may be

considered diagnostic. Isotopomers will be excluded unless they are characteristic of a specific

chemical composition. Normally this will be limited to chlorine and bromine isotopomers, but

other possibilities may arise. Ions resulting purely from a derivatizing or complexing reagent willnormally be excluded from the list of diagnostic ions. For example,themlz 73 ion of atrimethylsilyl derivative may not be chosen as a diagnostic ion. Normally the (pseudo)molecular

ion for a compound will be considered diagnostic, unless the intensity for that ion is less than 5%o

of the intensity for the base peak in the background-subtracted spectrum of the component in

question.

9.4 Determination of the "Base Peak" in a Mass Spectrum

The base peak for the mass spectrum of a known standard is the most intense signal for a

diagnostic ion in the background-subtracted spectrum. For the purpose of determining relative ion

intensities the base peak in an unknown mass spectrum will be taken as the base peak of the

standard spectrum to which it is being compared, even if a different diagnostic ion shows higher

intensity in that spectrum.

In instances where it can be demonstrated that the nominal base peak signal is significantlydisturbed by an uncorrectable chemical interference, the second most intense diagnostic ionpresent in the spectrum may be used as the base peak. Such interference will normally be

demonstrated by showing that a reconstructed ion trace for the ion in question is not coincident

with the traces for other ions associated with the component of interest.

9.5 Method for Calculating Ion Ratios

Ion ratios will normally be determined by integrating reconstructed ion traces for each diagnosticion present in a given component. All integrations of reconstructed ion traces from a given


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component should have comparable stop and start points. Ion ratios are then calculated bydividing the area for each ion trace by the area for the trace ofthe base peak ion, and expressing theresult as a percentage. In instances where the reconstructed ion traces produce non-integratabledata, it is acceptable to substitute ion abundances from the background subtracted spectrum of thecompound of interest for the integrated areas from reconstructed ion traces. This will normallyhappen in situations where multiple sorts of mass spectral data are simultaneously acquired in a

single analytical run, resulting in discontinuous data streams for the various individual massspectral experiments.

l0 Instrument Conditions

Not applicable.

1l Decision Criteria

Provided below are guidelines for establishing a match between a known mass spectrum and thatof an unknown spectrum. Note that some analytical standard operating procedures (SOP's)include detailed criteria for the evaluation of mass spectra of individual target analyes. Suchspecific instructions will supercede the guidelines provided below.

In almost all cases, unknown spectra should be matched against known spectra obtained fromcontemporaneously analyzed reference material. Exceptions are discussed in section 12.5 of these

guidelines. When assessing spectra for a targeted analyte from multiple unknown samples in a

single analytical run, it is acceptable to compare each unknown spectrum to the known spectrumresulting from a different contemporaneously analyzed reference sample. The mass spectra ofmany chemical entities are known to vary with analyte load. It is acceptable to dilute and

reanalyze a sample containing a high level of a suspected target compound in order to be able tomore appropriately match its spectrum to a lower concentration standard, control, or calibrator.

11.1 For Full Scan Mass Spectra

In order to establish a match between known and unknown mass spectra in the full scan mode, bothof the followine criteria should be met:

Every significant ion present in the known spectrum should be present in the unknownspectrum, and vice-versa.

All relative intensities for diagnostic ions in the unknown spectrum should match thoseobserved in the known spectrum within the tolerances shown in Table I or Table 2. Ifthese limits would produce an acceptable lower bound of less than lo/o for a given ion ratio,

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the lower limit will be set at 106. Ion ratios for specific diagnostic ions may be excludedfrom consideration if they meet any of the following criteria:

l. The ion ratio for that ion in the known spectrum is less than 5o/o (less than l\Yo forCI, ESI, or APCI spectra).The signal-to-noise ratio of the reconstructed ion trace for that ion in the unknownspectrum is less than 3.

It can be shown that the signal for that ion in either the known or the unknownspectrum is significantly disturbed by an uncorrectable chemical interference.Such interference will normally be demonstrated by showing that a reconstructedion trace for the ion in question is not coincident with the traces for other ions

associated with the component of interest.

If there are more than four diagnostic ions in the known spectrum, then the examiner need onlyevaluate the ratios for four diagnostic ions (three ratios) in order to establish a scientifically validmatch between the spectra. For compounds with a molecular weight less than 80 AMU, only three

diagnostic ions (2 ratios) need be evaluated to establish a scientifically valid match. The selected

ions will normally include the base peak and the (pseudo)molecular ion, unless those ions meet

one ofthe three exclusion criteria given above. If fewer than three diagnostic ions are available forevaluation, the specha may still be matched, but the examiner should be aware that the information

content derived from such a match is limited, and should be regarded with caution. Examiners

should also take care to ensure that the chosen scan range provides adequate "buffer space" around

the diagnostic and significant ions of the substance in question.

Matchi for CI. ESI. and APCI M

11.2 For SIM Mass Spectra

Selected ion monitoring experiments can allow for the detection of very low levels of analyte in

complex sample matrices, at the cost of reducing the information content of that experiment.Examiners should take great care in selecting monitored ions for a SIM experiment. Ions for aSIM experiment must be based upon a known full scan spectrum of the species of interest collected


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If the ion ratio in the knownspectrum is:

>5IYo >25o and <50% <2504

Then the ion ratio in the unknownsDectrum should be within:

l0% absolute 20%o relative 5% absolute

able 7: lon Ratto ln erances a ASS

If the ion ratio in the knownsnectrum is:

>60Vo >40Yo and <60%o <40%

Then the ion ratio in the unknownsnectrum should be within:

l5% absolute 25Vo rclative 10% absolute

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on the instrument to be used for the SIM experiment. Four diagnostic ions will normally beselected (three ions for compounds with a molecular weight less than 80 AMU; see 12.4 foranother exception), and, if possible, all should be significant as well as diagnostic. The base peakwill normally be one of the chosen ions, and the (pseudo)molecular ion should be included if it hasa relative intensity greater than 5o/o in the known full scan spectrum. In order to establish a matchbetween a known SIM spectrum and an unknown SIM spectrum, all resulting ion ratios shouldmeet the tolerances specified in Table I or Table 2, as appropriate.

11.3 For Tandem Mass Spectrometry (MS/LS)

Tandem mass spectrometry can lend a great deal of additional specificity to mass spectralexperiments by greatly increasing the confidence that the ions in a given spectrum are allassociated with a single substance. Due to the nature of most collision-induced dissociationprocesses, however, ion ratios in tandem mass spectra tend to be much less stable, and much moredependent on analyte load, than is true for classic electron impact mass spectra,

Tandem mass spectra tend to be much "cleaner" than full scan mass spectra, with fewer extraneousions. Therefore, the limit for determination of significant ions in a tandem mass spectrum islowered to l}Yo (from l5%) of the most intense observed ion in the background subtractedspectrum. The high probability of ion association in tandem mass spectrometry means that nearlyall ions of reasonable intensity observed in an MS/lvIS experiment should be considered diagnostic,with the exception of ions resulting purely from the loss of an adduct.

Due to vagaries of the physical processes involved in the precursor ion isolation and fragmentationevents in an ion trap mass spectrometer, tandem mass spectra acquired on such an instrument willoccasionally show an "ion-splitting" artifact for a precursor ion returned in a product ion massspectrum. This is evidenced by the presence of trvo ions, separated by a fraction of an AMU, at thenominal mass of the precursor ion in the product ion spectrum. In instances where thisphenomenon is observed, the response for the affected ion should be taken as the total of theresponse for both components of the "split" ion signal.

11.3.1 Product Ion Experiments

When conducting product ion experiments, the selection of a precursor ion is critical to obtaininguseful and reliable information. In most cases, the (pseudo)molecular ion of the species underconsideration should be selected, if available. It is also acceptable to use a diagnostic isotopomerof the (pseudo)molecular ion, if one is available. If the (pseudo)molecular ion is not available, oris not suitable for some reason, then the selected precursor ion should be both significant anddiagnostic in the full scan mass spectrum of the substance under consideration. With product ionspectra, it is also important to ensure that the observed fragment spectrum is, in fact, emergingfrom the selected precursor ion. For this reason, one of the fwo following criteria should normallybe met for a product ion spectrum:


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a. The precursor ion should be observed in the product ion spectrum with an ion ratio of at

least 5%.

b. If full scan mass spectral data are collected concunently with the product ion spectra, the

full scan spectrum of the component of interest should show no ions within 1.5 AMU of the

precursor ion with greater than three times the intensity of the precursor ion.

In order to establish a match between a known product ion spectrum and the product ion spectrum

of an unknown, both of the following criteria should be met:

a. Every significant ion present in the known spectrum should be present in the unknown

spectrum, and vice-versa.

b. All relative intensities for diagnostic ions in the unknown spectrum should match those

observed in the known spectrum to within the tolerances shown in Table 3. If these limits

would produce an acceptable lower bound of less than loh for a given ion ratio, the lower

Iimit will be set at0.5o/o. Ion ratios for specific diagnostic ions may be excluded from

consideration if they meet any of the following criteria:

1. The ion ratio for that ion in the known spectrum is less than 5%a.

2. The signal-to-noise ratio of the reconstructed ion trace for that ion in the unknown

spectrum is less than 3.

3. It can be shown that the signal for that ion in either the known or the unknown

spectrum is significantly disturbed by an uncorrectable chemical interference.

Such interference will normally be demonstrated by showing that a reconstructed

ion trace for the ion in question is not coincident with the traces for other ions

associated with the component of interest.

If there are more than three diagnostic ions in the known spectrum, then the examiner need only

evaluate the ratios for three diagnostic ions (two ratios) in order to establish a scientifically valid

match between the spectra. The selected three ions should include the base peak and the precursor

ion (if present), unless those ions meet one of the three exclusion criteria given above. If only a

singie diagnostic ion is observed in the product ion spectrum, spectra may still be matched, but the

.*u*in.r thould be aware that the information content derived from such a match is limited, and

should be regarded with caution.

ol for MS/lvlS Prod Ion S


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If the ion ratio in the known spectrum is: >400 s40%

Then the ion ratio in the unknown spectrum should be within: 25o/o relative l0% absolute

FBI LabordtoryChemistry Unit



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LL.3.2 Precursor Ion and Neutral Loss Experiments

The practical information content for precursor ion and neutral loss MS/lvIS experiments isgenerally low, but circumstances may stillarise in which one of these techniques can provide

critical additional information about a given substance. For precursor ion experiments, a match

between a known and an unknown spectrum may be established if all significant ions present in

the known spectrum are present in the unknown spectrum, and vice-versa. For neutral loss

experiments, a match between a known and an unknown spectrum may be established if all

significant transition pairs present in the known spectrum are present in the unknown spectrum

and vice-versa.

11.3.3 Selected Reaction Monitoring (SRM) Experiments

SRM analysis shares many features, advantages, and limitations with SIM analysis, but benefits

from the added specificify afforded by tandem mass spectrometry. Three diagnostic ion

transitions should be chosen for an SRM experiment. Generally, all three transitions should share

a common precursor ion, although it is appropriate to use multiple precursor ions if all are part ofa diagnostic isotope cluster in the full scan spectrum of the substance in question. It is desirable

that the chosen precursor ion be the (pseudo)molecular ion of the substance in question. If this is

not possible, or not practical, then the chosen precursor ion should be both significant and

diagnostic in the full scan spectrum of the substance in question. In order to establish a match

between a known SRM spectrum and an unknown SRM spectrum, both resulting ion ratios should

meet the tolerances specified in Table 3'

11.3.4 Higher Order (MS") Tandem Mass Spectrometry

Tandem mass spectra of order higher than2 are beyond the scope of this document. There is little

to no discussion of this subject in the various published technical guidelines, and the technique is

rarely practiced in forensic and regulatory settings. When used, higher order tandem mass spectra

will be addressed on a case-by-case basis, usually as a part of method validation. Examiners

should consider using the criteria for product ion MS/MS in section 12.3.1 as a starting point forsuch evaluation.

11.4 Exact (Precise) Mass Measurement Techniques

Exact mass measurement can provide a significant additional level of information content in a

mass spectrum, giving an examiner more confidence in any conclusions based upon that spectrum.

The use of exact mass measurement techniques does not, however, allow an examiner to disregard

other aspects of the mass spectrum under consideration. As such, mass spectra obtained using

exact mass techniques should still meet all of the matching criteria for the appropriate mass

spectral techniques given above, but different standards may be used in selecting diagnostic ions,

and more confidence can be placed in matches based upon a limited set of diagnostic ions.

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Revision: 0

Page9ofl5

Ions in an unknown spectrum willbe considered to be an exact mass match to those in a knownspectrum if the measured masses agree to within 0.005 AMU. For a SIM experiment, only threeions, instead of four, need be monitored, and show appropriate ion ratio agreement, if all three ionsmeet this exact mass match criterion. When determining diagnostic ions, any isotopomer of a(pseudo)molecular ion may be considered diagnostic if it meets this exact mass match criterion.One additional adduct ion, beyond the pseudomolecular ion, may also be considered diagnostic ifit meets this exact mass match criterion.

11.5 Matching to Library Spectra

While mass spectral libraries (either commercial compendia or collections generated in-house)can be invaluable tools in helping to direct examinations and suggest possible targets for furtherinvestigation, an examiner should remain aware of the limitations of these libraries, Mostcommercial libraries do not clearly indicate the instrumentation the spectra were acquired on, orat what level of sample loading. In-house library data may have been acquired on the sameinstrumentation used to obtain a given unknown spectrum, but it is very difficult to ensure thatlong-term drift in instrument performance has not compromised the reproducibility of thoselibrary spectra.

Despite these limitations, there may arise rare instances in which it is necessary to compare anunknown spectrum to a library entry, for example if a standard of the substance in question cannotbe readily obtained, or for purposes of screening to direct further investigation. In cases wheresuch matching is attempted, all criteria for the appropriate type of mass spectrometry, given above,should still be observed, with one significant change. In these instances, ion abundances for thedetermination of ion ratios will be measured as the intensity of the ion in the spectrum, rather thanas the integrated area of a reconstructed ion trace. For the unknown spectrum, all criteriaregarding averaging and background subtraction from section 10.1 should still be observed.

12 Calculations

IR* : (A*/A6)xl 00%, where:

IR* = the ion ratio for ion xA* : the integrated area of the reconstructed ion trace for ion x4,6: the integrated area of the reconstructed ion tpace for the base peak ion(lon abundances from background subtracted mass spectra may be substituted for integrated areasunder certain circumstances detailed in section 9.5.)


Not applicable.


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Revision: 0Page l0ofl5

14 Limitations

This procedure, while extensive, is not intended to be exhaustive, and situations will arise in whichtheir blind application could lead to inappropriate conclusions. No set of rules can ever replace thegood judgment of a trained and experienced examiner. The mere fact that an unknown massspectrum matches wellto the spectrum of a known standard will rarely, by itself, be sufficientgrounds to claim the presence of that compound in the questioned sample. All of the analyticaldata for the samples in question should be considered when drawing such final conclusions.Similarly, the fact that an unknown mass spectrum fails to match that of a known standardgenerally will not, by itself, constitute grounds for concluding that the compound is not present inthe questioned specimen.

This protocol does not excuse an examiner from exercising care in the acquisition of mass spectraldata. It should be remembered that poor practices in the acquisition of mass spectra willyield datathat is useless at best, and misleading at worst. Samples that show evidence of severechromatographic overload should generally be diluted and reinjected in order to obtain reliablemass spectra. Instrument calibration is also critical for obtaining useful mass spectral data, and itis incumbent upon any examiner to run appropriate test samples to demonstrate proper instrumentfunction.

15 Safety

Not applicable.

16 References

Betham, R.,; Boison, J.; et al J. Am. Soc. Mass Spectrom.2003,14,528-541.

deZeeuw, R. A. I Forensic Sci. 2005, 50,745-747.

Mclafferty, F. W.; Stauffer,10. t229-1240.

Soc. Mass Spectrom. 1999,

A. Forensic Sci. Int. 2004. 145.85-96.

deZeeuw, R. A. -r. Chrom. B 2004,811, 3-12.

Technical Document TD2003IDCR, 2004; World Anti-Doping Agency, Montreal, Canada.

Bowers, L. D.; Armbruster, D.A.; et aINCCLS DocumentC43-A,2002:The NationalCommittee


Ev ?ub(at'\



lssue Date: 06/21/06Revision: 0

Page ll of15

for Clinical Laboratory Standards, Wayne, PA.

Instrument Operations and Support Subunit SOP Manual,


fi uvu(s"")

liBl l.aboratorrChemistry Lrrrit

Toxicology Suhunir'l ox I0'1-0.doc

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0621n6 Original Issue

ADnrovrrl

crrenristry Llnit chier: 4//O*q{}-.*--Marc r\. LeBeau

OA Approval

Quality ivlanager:

Issuance

Tox Subunit !{ar:ager :


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Appendix l: Mass Spectra Key Points

l. AveraginglBackground Subtraction of Mass Spectra: (* = subtracted spectrum)a. <6 scans averaged for sample (N)b. <2N+l scans for backgroundc. background outside area integrated for ion ratios

2. Significant Ions: Ion signal > l5o (10% for MSA4S) of most intense ion signal (*)

3. Diagnostic Ions (determine from mass spectra of known standard):a. Characteristic of chemical compounds chemical structureb. Diagnostic criteria (not well defined):

(Pseudo)molecular ion is diagnostic if intensity > 5% base peak (*)c. Non-diagnostic ions (generally exclude):

Adduct ions except pseudomolecular ionIsotopomers except chlorine and bromine isotopomersIons 2nory to a derivatizing reagent (e.g. m/z 73 TMS deriv)

4. Base Peak (determined from mass spectra of known standard):a. Most intense signal for diagnostic ion (*)b. Base peak standard is base peak unknown (Exception: can use second most intense

diagnostic ion if base peak has an uncorrectable chemical interference)

5. Method for calculating relative ion intensities:a. Determine ion abundances = integrate RIC's / EIC's for each diagnostic ionb. Integration - comparable stop & start pointsc. Ion ratios (expressed as o/o) = each ion trace area/base peak ion aread. Spectral peak height may be substituted for integrated area if the RIC data in

non-integrable.

6. Decision Criteria: Unknown spectra matched against known spectra.

6.1 Full Scan Mass Spectraa. Every significant ion in known spectra present in unknown and vice-versab. Relative ion intensities (EI)

Known Ion ratio > 50yo - unknown l0% absoluteKnown Ion ratio 25-50% - unknown 20%orelativeKnown Ion ratio <25yo - unknown 5% absolute

c. Relative ion intensities (CI, ESI, APCI)Known Ion ratio > 600A - unknown 15% absoluteKnown Ion ratio 40-60% - unknown 25YorelativeKnown Ion ratio < 40Vo - unknown 10% absolute


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Page 14 of I 5

6.2 SIM Mass Spectraa. Four diagnostic ions (three for compounds <80 AMU), all should be significantb. Base peak one ofthe chosen ionsc. (Pseudo)molecular ion RI > 5%d. Meet relative ion intensities

6.3 Tandem MS (ion ratio dependant on analyte load, less stable)a. All ions of reasonable intensity are diagnostic (Exception 2ndv loss of adduct)

6.3.I Product Ion (Daughter Ion) Experimenta. Select precursor ion (parent ion):

(Pseudo)molecular ion or one of its isotopomersb. Product spectra:

Precursor ion observed with ion ratio >5% OR full scan show no ionswithin 1.5 AMU of precursor ion with > 3x intensity of the precursor ion

c. Comparing product spectra (Standard to unknown = std to unk)Significant ions present both std and unkIf > 3 diag ions -need only ratio 3 diag (2 ratios)Ion ratios:

Known > 40yo - unknown 25%o relativeKnown < 40Yo - unknown l0% absolute

Exclude ion ratios if:Ion ratio known < 5olo

Signal-to-noise RIC unknown < 3Chemical interference in ion

6.3.2 Precursor ion and Neutral loss - must match stds with unknowns

6.3.3 Selected Reaction Monitoringa. 3 diagnostic ion transitionsb. Share common precursor ion, except isotopomer clustersc. Ion ratios:

Known > 40yo - unknown 25%orelativeKnown < 40o - unknown l0% absolute

6.4 Exact Mass (Accurate Mass)a. rn/z < 600: Std to Unk measured masses within 3 mAMUb. m/z> 600: Std to Unk measured masses within 5ppmc. SIM: only 3 ions need monitoring, in correct ratiosd. If above criteria is met:

Can use (pseudo)molecular ion if < 5% zuCan use any isotopomer of (pseudo)molecular ion


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'#l!'lii3can use up to one additional adduct ion, beyond pseudomorecular ion

Appendix 2: Glossary of Terms

Adduct Ion - Any ion to which another chemical entity has been attached by a means other thancovalent bonding.

Base Peak - The most intense or abundant diagnostic ion in the mass spectrum of a substance.

Diagnostic Ion - Any ion observed in the mass spectrum of a substance that is characteristic of thechemical structure of that substance.

Ion Ratio - The relative abundance or intensity of t'wo ion signals in a mass spectrum.

Isotopomers - Two or more chemical species that differ only in isotopic composition. Forexample, CH3OH and CD3OH are two isotopomers of methanol.

Molecular Ion - A charged intact molecular species, with charge acquired solely through the gainor loss of electrons. Normally denoted as M* or M- for singly charged species.

Precursor Ion - In tandem mass spectrometry, the ion selected for fragmentation. Often refenedto as a "parent ion",

Product Ion - In tandem mass spectrometry, an ion resulting from the fragmentation of another ion.Often refened to as a "daughter ion".

Pseudomolecular Ion - A charged molecule in which charge has been acquired through adductionof an ion or through loss of a moiety able to dissociate in solution. Examples include (M+H)*,(M-H)-, (M+Na)*, and (M+NHa)+.

Reconstructed Ion Trace - A display of the abundance or intensity of a single ion signal as afunction of time during an analysis. Often also called an "extracted ion chromatogram" (EIC) or"reconstructed ion chromatogram" (RIC).

Significant Ion - Any ion in the mass spectrum of a substance present above a specified intensityor abundance.


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VALIDATION

iio +4+.

Gr)

Chemistry UnitMethod Validation Review Form

This method has been appropriately validated for its intended use (as specified above). The method is considered fit for theabove use.

Unit Chief Approval:

ProcedureName: Arur,ysrs o7 EwA nt Dprrn Fuoogrr^,n,

tr Measurement of PhysicaUChemical Property

p/ nstablishment of Presence/Absence of Specific Analyte(s)/Class(es)

tr Quantitation of Specified Analyte(s)

g/ Selectivtty: Analysis of at least l0 sources ofblankmatrix + 2 zero samples (blank matrix spiked withinternal standard). Analysis of samples spiked withother compounds expected to be in real samples.

n Calibration Model Qinearity)..Analysis of at least5 non-zero calibrators at a minimum of 5 replicatesper level,

n Bias, Repeatability, and Intermediate Precision:QC samples at low and high conc in calibrationrange. Analysis ofduplicates ofeach conc in at least5 runs,

Limit of Detectioz; See Procedure for details.

tr lpwer Limit of Quantitation: See Procedure fordetails.

g/ UooX t6rcts.'For LC-MS(-MS) procedures only.Analysis of5 neat standards and 5 blank extracts

zltLldt,zlBloz

Additional Comments:

fi vuuftoa)

ltDate: 7/l'' / 07

-

METHOD

{^r V4Lr(^rr)

Instrument Method: EDTA pos Swabs.meth

LCQ fnstrument Method

Creator: AdminislratorLast modified: 2/12/OZ by AdministratorMS Run Time (min) : L0.00

Divert Valve: not used during run


Segment l_ fnformation

Duration (min) : l_0. 00Number of Scan Events: l_

Tune Method: EDTA_pos_CID

Scan Event Details:1: Pos . (293.0)->o(fZS.O-3j_5.0)

MS/MS: CE 15. 0? IsoW l_.0

Monday, February 12, 2OO7 12:55:05 page 1 of 2

{-v q4 c./;"s)

Injector parameters:Syringe draw rate (pl/sec)Injection volume (UI) :5

Pump settings:.Solvent A:5:95 ACN:Water +Solvent B:BSolwent C:CSol-vent D: D

Min pressure (pSI):0Max pressure (PSf) :5000Chart output: PressureChart output:Normal

Gradient program:Time (min) Flow (nl/min)

Waters 2690 LC Systern

:2.50

0.06t NH40H

0. 003. 00

0.300.30

A(*) B(t) c(t) D(t) Curve100.0 0.0 0.0 0.0 Linear1,00.0 0.0 0.0 0.0 Li_near

-6-6


Switch L:No changeSwitch 2:No changeSwitch 3:No changeSwj-tch 4:No change

Time(min) EvenE0. 00 Switchl

Action ParameterNo change

InsLrument Method: EDTA pos Swabs.meth

Monday, February 12, 2007 12:55:05 page 2 of 2

Z'v VVc'/ at ri\

fnstrument Method: EDTA Pos Swabs.meth

LCQ Instrument Met.hod

Creator : AdministratorLast modified 2/9/ 07 by Administrator

MS Run Time (min) : 10.00



Segment 1 Information

Duration (min): 10.00Number of Scan Events: 2Tune Method: EDTA_Pos_CID

Scan Event Details:l-: Pos - (293.0)->o(tZS.0-315.0)

MS/MS : CE 1-5. 0? IsoW 1.0

2: Pos . (305.0)->o(tZS.0-31_5.0)MS/MS : CE l-5. 0e IsoW 1. 0

(0", v,trn.,>) Ap

L2246242

f-<. q(u( ato\

Friday, February 09, 20A7 Page I of 2

InsLrument Met.hod: EDTA_Pos_Swabs . meth


Injector parameters:Syringe draw rate (pl,/sec) :2.50Tnicnf inn rrnl"-o /"I\,q"vrsne (pL) :5

Pump settings:Solvent A: 5: 95 ACN: l,f ater + 0 . 06* NH4OHSolvent B: B

. S6l \t6hf a. n

Solvent D: DMin pressure (pSI):0Max pressure (pSI) :5000Ch: ri ^rrf nrlf . D-_. - -essureChart output:Normal

Gradient program:Time(min) Flow(mI,/min) A(t) B(E) C(t) D(E) Curve0.00 0.30 100.0 0.0 0. 0 O . 0 Linear _ 63. 00 0 . 30 100.0 0. 0 0. 0 O. O Linear _ 6

Timed events:Tn i f i a l qt- ri6a.

Switch L:No changeSwitch 2:No changeSwitch 3:No changeSwitch 4:No change

Tj.me (min) Event Act j.on parameter0. 00 Switchl No change

Friday, February 09, 2OO7 12:46:42

&qq6( st,\

Page 2 of 2

METITOD

4 ,/qb1; r-t)

Instrument Method: EDTA Neq Swabs.meth

LCQ Instrument Method

Creator : AdministratorLast modified: 2/9/07 by AdministratorMS Run Time (min) : 10.00


MS Detector Sett.inqs:

Segrnent I Information

Duration (min) : l-0.00Number of Scan Events: 4Tune Method: EDTA_NEG

Scan Event Details:l: Neg - (291.2)->oS (246.5-247.5 272.5-273.5)

MS/MS: CE 15.0? Isow 1.0

2: Neg . (303.2)->oS(292.8-284.3)MS/MS : CE l-5. O? IsoW 1. 0

3: Neg . (344.2)->oS (299.5-300.5 325.5-326.5)MS/MS: CE 15.0? rsow 1.0

4: Neg - (356.0)->oS(31j-.5-312.5)MS/MS: CE 15. O? IsoW L. 0

2007 12:47:03

f-x (qa(at z\

Friday, February 09, Dana 1 n€ argYU + v! a

Instrument Method: EDTA Necr Swabs.meth


lnjector parameters:Syringe draw rate (F1lsec):2.50fnjection vol-ume (p1) :5

Prrmn c6f l- i nfic .

Solvent A:80:20 ACN:Water + 0.03t NH4OHSoLvent B:BSolvent C:CSolvent D:DMin oressrrrc lPSf):0Max pressure (PSI) :5000Chart output: PressureChart output:Normal

Gradient program:Time(min) Flow(ml,/min) A(t) B(t) C(E) D(t) Curve0.00 0.30 100.0 0.0 0.0 0.0 Linear - 63.00 0.30 l-00.0 0.0 0.0 0.0 Linear - 6

Timed events:Tni ii r1 ei-rl-oc.

Switch L:No changeSwltch 2:No changeSwitch 3:No changeSwitch 4:No chanoe

Time (min) Event Action Pararneter0.00 SwitchL No chanqe

Friday, February 09, 2007 1-2247 203 page 2 of 2

a4 lqb/t> u\

SELECTIVITY

fu 44b(^r t)

tSample Name:

C- nent:

Seq uence---select_pos. sld [O pen]

A, Case 1, Grey

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type Ftle Name Sample lD Path

Unknown SELOl 1 C:\)(calibuAData\EDTA\BreweASEL Positive

Inst Method Proc Method CalFile Position InjVol Level Sample WtC:Xcalibur\methods\EDTA Pos Swabs 1 5.0 0.000


0.000 0.000 1.000

*****************************i*****i**t********+********************************i*******t*t***tt**i***********t*********

Sample Name: Swab.A, Case 2, Red

Comment: Study:

Client:

Laboratory:

Company:

Phone:


Unknown SELO2 02 C:Xcalibur\Data\EDTA\BreweASEL Positive

Inst Method Proc Method Cal File Position InjVol Level lSample Wt

C:Xcalibur\methods\EDTA Pos Swabs 2 5.0 0.000


0.000 0.000 t.00u

/* q+b1; t,')page 1

6uzf t lot

Sample Name:

C' -nent:

Seq uence--select_pos. sld [Open]

Swab B, Case 2, Grey

Study:

Client:

Laboratory:

Company:

Phone:


Unknown SELO3 03 C:U(calibur\DataEOtffi


0.000 0.000 1.000

*t**t**t**********ii*t***********t**t*****************************t*****ti****i***tr****t*******th*r

Sample Name:

Comment:

Swab C, Case 3-1, Grey

Study:

Client:

Laboratory:

Company:

Phone:

iample Type File Name Sample lD Path

Unknown lSEL04 04 C:Xcalibur\Data\EDTA\Brewer\SEt positive


0.000 0.000 1.000

*******************t*************i**************tt*t*******t******t***********t****************t******************ffi***********************

{" q4e,( nt)

6vzf rl.t

p

Sample Name:

/--lment:

Sequence--select_pos. sld [Open]

Swab C, Case 3-2,

Study:

Client:

Laboratory:

Companyi

Phone:

Sample Type File Name Sample lD PathUnknown SELOs 05 u : \Acail0u nData\E DTA\B reweAS EL_positive


******t*t***i*ti**********i*****t*********t**********************t******************************************H****************r********ttt*t***

Sample Name:

Comment:

Swab

' Study:

Client:

Laboratory:

Company:

Phone:


***t**t*i***t*t*t********i**********************+*****************a*************************i*******t*************************************t***

4(a

ffizlnl'trylu

)s)

Sample Name:

C' rent:

Seq uence---select_pos. sld [Open]

b D, Case 3*4,

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD

Unknown SELOT 07 C:XcalibuAData\EDTA\BreweASEL Positive

Inst Method Proc Method Cal File Position InjVol Level Sample WtC:XcalibuAmethods\EDTA Pos Swabs 7 5.0 0.000


0.000 0.0rJ0 1.000

Sample Name:iSwab D, Case 4-1, Red

Comment: Study:

Client:

Laboratory:

Company:

Phone:


unKnown SELOS 08 C:U(calibur\Data\EDTA\Brewer\SEL Positive


u:v(calrbur\metnods\tu lA Pos swabs I 5.0 0.000


0.000 0.000 1.000

6r{o qq, >lnln(an)

Sample Name:

C- rent:

Seq uence---select_pos. sld [Open]

, Case 5, Red

Study:

Client:

Laboratory:

Company:

Phone:


Unknown SELOg 09 C:\XcalibuAData\EDTA\BreweASEL Postlive

Inst Method Proc Method CalFile Position InjVol Level Sample WtC:\Xcalibur\methods\EDTA Pos Swabs I 5.0 0.000


0.000 0.000 1.000

Sample Name:

Comment:

ellow

*t***********t**i**tt**********t**********************s******s***i********rl***********

Study:

Client:

Laboratory:

Company:

Phone:


Unknown SELlO 10 C:Xcalibur\Data\EDTA\Brewer\SEL Positive

Inst Method Proc Method Cal File Position lnjVol Level Sample Wtu:u(cattbunmethods\EDTA Pos swabs 10 5.0 0.000


0.000 0.000 1.000

{v a4 r- Ll,fu( axc)

Seq uence--select_pos. sld [Open]

Sample Name:

C- 'nent:Swab A, MAL, Yellow, d

Study:

Client:

Laboratory:

Company:

Phone:


Unknown SELl 1 11 C:U(calibur\Data\EDTA\Brewer\SEL Positive

Inst Method Proc Method Cal File Position lnjVol Level Sample WtC:Xcalibur\methods\EDTA Pos Swabs 11 5.0 0.000


U.UOO 0.000 1.000

Sample Name:

Comrnent:

*tl**********************t******t****t*********t**i**************************t**t********t***************

Swab D, MAL, Yellow, d12

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD ath

Unknown SEL12 12 C:Xcalibur\Data\EDTA\Brewer\S EL Positive

lnst Method Proc Method CalFile Position njVol Level Sample WtC:Xcalibur\methods\EDTA Pos Swabs 12 5.0 0.000


0.000 0.000 1.000

t. qq u(1u,1

{eul tl't

.,, i*,a,ru, 0...r. e l-eo, itiu(Gi]\ 02109107 10:57:05 1 SwabA, Cdsdl.ErEV--.r- ____1 /

1812.57

1 00-l

go-.1

I

NL:4.76E3rn/z='159.S160.5 .

F: + c ESI Full [email protected] [125.00.315.00t MSSet0l

Selul*/5-96 RI: 0.96-1.27 AV: 12 NL:8.71E3F: + c ESI Full ms2 [email protected] [ 125.00-315.00]

erurF64-1ul Kt:1.',Iu-1.3'l AV:9 NL: 1.16E4: + c ESI Full ms2 [email protected] [125.00-315.001

ntlz= 246.5-247.5F: + c ESI Full [email protected] [125.00-315.001 MSSelOl

m/z= 167.t168.5F: + c ESI Full [email protected] [12s.00.315.001 MsSelo1

8.28E3

6.46E3rn/z= 258.$259.5F: a c ESI Full [email protected] [125.00-31s.001 MsSel0'l

NL:6.89E4TIC MS Sel01

o

6E

o

Go

ooco

o

-s!od

L,t 4(a

NL:4.76E3m/z= 159.5-160.5F: + c ESI Full [email protected] [125.00-315.001 MSSel01

mlz= 246.5-247.5F:+ c ESlFull [email protected] [12100-315.001 MS

miz= 167.5-168.5F: + c ESI Full [email protected] [125.00-315.001 MSSel01

mlz= 258.5-259.5F:+ c ESI Full [email protected] [125.00-315.001 MSSel01

TIC MS Sel01

f.'L+u

2773.63197

2.58

q.,

.zoEx.

Tima /minl (av t\

0?/09107 10:57:05 atr(el01#E4-87 RT: 1.11-1.14 AV: 2 NL: 6.7SE3-: + c ESI Full ms2 [email protected] [ 125.00-315.00]NL:1.37E3

m/z= 159.$160.5F: + c E5; 5u1 .",[email protected] I125.00-315.001 MSSel01

o

GE

o

o

@0

: + c ESI Full msz [email protected]

oo6u

o=.go6.03E4

rnlz= 167.5.168.5F: + c ESI Full [email protected] [125.00-3'15.001 MSSel01

NL: 2.93E4125.00-31s.001

TIC MS Sel01

C :U(qalibur\...\Sel-PositivEffi)n_ \-1 0U09107 10:57:05 A, Case 1, Grey aapNL: 1.37E3rniz= 159.S160.5F: + c ESI Full [email protected] I125.00-315.001 MSSelol

Sel01#90-95 RT: 1.19-1.24 AV:3 NL: 1.16E4F: + c ESI Full ms2 [email protected] [ 125.00-315.001

+ c ESt Fult ms2 [email protected] 12s.00-315.001

.ll'lz= 246.5-247 ,5F: + c ESI Full [email protected] [125.00.315.001 MS

6.1 9E3

:9.ZJEJ

oo6!a!o

oo

oo6E

0

6o

rn/z= 258.5-259.5F: + c ESI Full [email protected] Ir25.00-315.001 MsSelo1

NL:6.03E4TIC MS Selol

6,t

n/z:167.5-16E.5F: + c ESI Full [email protected] ['125.00-3't5.001 MsSel0'l

(as

02109107 11:08:17 Swab A, Case 2, Red

rlz= 246.5-247.5F: + c E51 Pu11 *,[email protected] [12100-315.00] MS

NL:7.66E3rn/z= 258.5-259.5F: + c ESI Full [email protected] [125O0-315.001 Ms

oooE

o

6o

o

6

o.=

"g!o

tb

)

1+ c ESI Full ms2 [email protected] [ 12S.OO-glS.OO]

NL:6.62E4TIC MS Sel02ro0l

,o-]

*.1

ro-l

uo-l

170z.1J

6,/

NL:0rvz= I 59.5.1 60.5F:+q551 [email protected] [125.00-315.00r MSSelo2

: + c ESt Fuil ms2 [email protected] [ 125.00-315.001

2'?6 nz

1841

200

158

r.-/5

. C:Vcalibur\...rSel-eositiv@lD 02109107 1 1 :19:06 -l0E

NL:0rvz= 159.5.160.5F: +c95; 6u1,r.,[email protected] [125.00-315.001 MSSel03

rnlz= 246.5-247 .5F:+cESl [email protected] MSSel03

trVz= 157.5.168.5F: + c ESI Full [email protected] [12100-315.001 Ms

ooG

-o':.s!o

r/z= 258.$259.5F: + c ESI Full ms2

?33.339i;trt*

2.51E3

: 2.99E4TIC MS Sel03

{.v

o

oE

o.=66

Swab B, Case 2, Grey

tuJrcz-tu Kt: u.6z{r.9u AV: 4 NL: 0+ c ESI Full msz 293.00@'t5.00 [ 125.00-315.001

uJ#62-6C Kt: l.Uir-].10 AV: 2 NL: 2.ggE3+ c ESI Full ms2 [email protected] [ 12S.OO-315.00]

LqJ

C :U(na I ibu r\...\SEL-Positiv(@ 0U09107 11:29:58

NL:0rn/z='159.5.160.5F: + c ESI Full ms2

i!"3#.9t33&r*

tnlz= 246.5-247 .5F: + c ESI Full [email protected] I125.00-315.001 Ms

r/z='167.5.168.5F: + c ESI Full [email protected] [

33r5d!0-31s.001 Ms

ooou!oo

.s!o

r/z= 25E.5-259.5F: + c ESI Full [email protected] [125.00-3't5.00t MsSetM

{nu(as

oooE4o,z

E

_--'( Swab C, Case 3-1, Grey)--__-_____-_-j-

tu4*ttz-tu Rt:0.62.0.90 AV:4 NL:0+ c ESI Fuil ms2 [email protected] [ 125.00-315.001

I+ c ESI Full ms2 15.00 [125.0G315.00]

0?J09rc7 11:40:49

NL:O lF; + crU X I: U.62.{J.9U AV: 4 NL: OFull ms2 [email protected] [ 125.00-31S.00]

rvz= 159.5-'160.5F: + c ESI Full ms2

ffi81319'ir"'

nr/z= 167.$'168.5F: + s E51 Prt r.,

i:fig3eJifir".

;;dii;ljri'!2-ift :d;6"is.,jt'r12s.00-3is.oot

mts= 258.$259.5F: + c ESI Full [email protected] [12100.315.001 MS

z--T':^)uv

oooo

o.=oo

1.1 3E5MS Sel05

o

o

o66

&,(at

C:\Xcalibur\...\SEL PositivI 0?J09107 11:51:40 ----<--)

)t)NL: O

m/z= 159.5-160.5F: + c ESI Full [email protected] t12s.00-315.001 MsSel06

o

EoJ

o6o

rn/z= 167.5,'168.5F: + c ESI Fult [email protected] t.

32",5d30-3 t s. ool' r,ls

efub*rur-r/6 Rr: 2.11-2.31 AV: 16 NLi 6ZSE: + c ESI Full ms2 [email protected] 1 rzS.oo:eiS.oOl

m/z= 256.$259.5F: + s E51 Prt rs2

U3;l3e;3f3rr^

NL: 1.37E5TIC MS Sel06

ooo

oo

6

'u xt; u.bz{J.gu Av:4 NL:0Full ms2 [email protected] [ i25.00-31S.00]

. C:U(calibur\...\SEL 0U09lO7 12:02:31 Swab D, Case 3-4,

T: + c ESI Full ms2 [email protected] t 125.06iJ

-YrFNL:0rn/z= 159.5-160.5F: + c ESI Full [email protected] [12s.00-315.001 MsSel07

IG

4

o

l9o

'NL: 1.25E5TIC MS Sel07

o

ou

o

.s!o

fo'/

utnz-tv r t; u.6z-u,9u AV: 4 NL: 0+ c ESt Fuil ms2 [email protected] [ 125.00-315.00I

fil/z= 167.t168.5F: + c ESI Full ms2305,[email protected] [12530-315.001 Ms

rn/z= 258.S259.5F: + c ESI Full ms2

?3*339t33&r",

( aq,

, C:U(calibun...\SEL positive{ffi;)t- OZ09l07 12:.13:2'l an

NL: 0n/z= 159.$160.5F: + c ESI Full [email protected] [125.00-3't5.001 MSSel08


c)ooE

o.a.go

ruz= 167.$168.5F: + c ESI Full [email protected] [12100-315.001 Ms

m/z= 258.$259.5F: + c ESI Full [email protected] ['125.00-315.001 MS

736 Sel089.68

NL:'1,15E5TIC MS Sel06

ooo

o.:so

r c ESI Full ms2 [email protected] [ 125.00-3tS.O0l

6,

NL:0rn/z= 159.5-160.5F: + c ESI Full ms2.Yr.uu(4 to.uu t125.00-315.001 MSSel09

8.85 n:/z= 246.5-247 .sI F: + c ESI Full ms2

[email protected] |125.00-31 5.001'Ms

ntz= 25E.5-259.5F: + c ESI Futt [email protected] t12100-315.001 Ms

+ c ESt Fuil ms2 [email protected] [125.00-315.001

Full ms2 [email protected] [ 125.00-31S.00]

TIC MS Sel09

02t09t07 12..35..M Swab A, MAL. Yellow

trVz= 159.$160.5F: + c 551 Pr;; t",[email protected] I125.00-315.001 MS

: E. l4E3fil/z= 246.5-247.5F: + c ESI Full ms2

?i3:33913331t*

0o6E

o.:6o

1001

'o-]

'o-l. ,n_j

100-l

go-l

*-l,^l'"tuo-]

t" qq

+ c ESI Fuil msz [email protected] [ 125.00-315.001

9.97E2nvz= 'l 67.5-1 68.5F: + c ESI Full ms2

j!fli&ets,lerr*

m82 [email protected] [ 125.00-315.001

1 9a rso

168

182

't8/.

144

1

( aq+

rXcalibuA...\SEL-eo.itiu@ 0?/09107 12:45:5,4

{bFnvz= 159.$160.5F: + c ESI Full [email protected] [125.00-315.001 MS

rtlz=246.5,247.5F: + c ESI Full [email protected] [125.00-315.001 MSSalt'l

. a ddtrt

IoE

oooEu

MS SelllNL:Ilc

rn/z= 258.$259.5F: + c ESI Full [email protected] [125.00.315.001 MSSel1l

fr'l(

I6u€o

66

Swab A, MAL, Yeltow, OiZ spifea-\

: + c ESI Fuil ms2 [email protected] [ 125.00-315.00]

[ 125.00-315.001

i.94 150

(v

02109107 12:57:01 "TI'FNL:0rn/z= 159.$160.5F: + c ESI Full [email protected] ['125.00-315.00t MSSel12

+ c ESI Full ms2 [email protected] [ 1

et14t4-tI Kr: U.97-l.OO AV: 2 NL: 1.22E4: + c ESt Full ms2 [email protected] [125.00€15.00]

'Itlz= 246.5-247.5F: + c ESI Full [email protected] [125.00-315.001 MSSel12

!)

6

f!

ooo

o

oEoo.z6o3.0'1E5

MS Sel12100-]

;l--lza)-luo-]

dz= 258.$259.5F:+cESl [email protected] [125.00-315.001 MSSel l2

Seq uence--select-neg. sld [Open]

Sample Name:

c '"nent:

Swab A, Case 1,

Study:

Client:

Laboratory:

Company:

Phone:


Unknown Sel01 1 C :Xcalibur\Data\EDTA\Brewer\S E L_Negative


C:U(ca I i bu r\methods\EDTA-Neg-Swabs 1 5.0 0.000


0.000 0.000 1.000

Sample Name:

Comment:

, Case 2, Red

Study:

Glient:

Laboratory:

Company:

Phone:


Unknown Sel02 02 C : Xcal i bu AData\EDTA\Brewer\S E L_Negative

lnst Method Proc Method Cal File Position InjVol ,Level Sample Wt

C : U(ca li bu r\method s\EDTA_Neg_Swabs 2 5.0 0.000


0.000 0.000 1.000

*****tt***********t***********************#**********t***r**********

,49;r*u'

C"+4a( att)paqe 1

Sample Name:

C rent:

Seq uence---select_neg. sld [O pen]

Swab B, Gase 2,

Study:

Glient:

Laboratory:

Company:

Phone:


Unknown Sel03 03 C:Xcal ibu r\Data\E DTA\BreweASEL_N egative

lnst Method Proc Method Cal File Position lnjVol Level Samole Wt

C : Xcalib u Amethods\EDTA_Neg-Swabs 3 5.0 0.000


0.000 0.000 1.000

Sample ttame:

Comment Study:

Client:

Laboratory:

Company:

Phone:

Type File Name Sample lD Path

Unknown Sel04 04 C :U(calibu r\Data\EDTA\Brewer\S E L_N egative

nst Method Proc Method CalFile Position InjVol Level rSample Wt

C :U(ca li bu r\methods\EDTA-N eg-Swabs 4 5.0 0.000

Sample Vol ISTD AMt Dil Factor

0.000 0.000 1.000

4rtt*t"€, ++,-lrq s)

Sample Name:

r .ment: Study:

Client:

Laboratory:

Company

Phone:

Seq uence--select_neg. sld [Open]


Unknown Sel05 05 C:Xcalibur\Data\EDTA\Brewer\SEL Neqative

Inst Method Proc Method Cal File Position InjVol Level Samole WtG:Xcalibur\methods\EDTA Neo Swabs 5 5.0 0.000


0.000 U.OUO 1.000

Sample Name:

Comment:

Swab C,

Study:

Client:

Laboratory:

Company:

Phone:


unKnown Sel06 06 C :Xcal ibu AData\EDTA\BreweAS EL_Negative

Inst Method Proc Method Cal File Position InjVol Level ]Sample WtA_Neg_ 6 5.0 0.000


0.000 0.000 1.000

+t

44uaq ri\

oJf'

Sample Name:,Swab D, Case 3-4, GreY

Sequence--select-neg. sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:

(' rent:


Unknown Sel07 07 C :Xcal ibu r\Data\E DTA\Brewer\SE L-Negativg


C : U(cal ibu r\meth ods\E DTA-Neg-Swabs 7 5.0 0.000


0.000 0.000 1.000

Sample Name:

Comrnent:

Swab D, Case 4-1,

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name lSample lD Path

Unknown Sel08 08 C :\)(cal ibu r\Data\EDTA\B rewer\SEL-Negative


C :U(ca li bu r\method s\EDTA-Neg-Swabs I 5.0 0.000


0.000 0.000 1.000

ty- 4ab/s"9

r\'('u4 M

,-|'

Sample Name:

r nent:

Seq uence--select-neg. sld [Open]

D, Case 5,

Study:

Client:

Laboratory:

Company:

Phone:


Unknown Sel09 09 C :Xcalibun\Data\EDTA\Brewer\SEL-Negative


C :U(cal i bur\methods\EDTA_Neg_Swabs I 5.0 0.000


0.000 0.000 1.000

Sample Name:lSwab A, MAL, Yellow

Comment: Study:

Client:

Laboratory:

Gompany:

Phone:


Unknown Sel10 10 C : U(calibu r\Data\E DTA\Brewer\S E L-N eg ative


C :U(cal i bu r\methods\EDTA-Neg-Swabs 10 b.0

Sample Vol ISTD AMt DilFactor

0.000 0.000 1.000

L,{ L{+(-/^ \( Joi)

*Jt*,"

Seq uence--select_neg. sld [Open]

Sample Name:

t' 'ment:

A, MAL, Yellow, d12

Study:

Client:

Laboratory:

Cornpany:

Phone:

sample lype File Name Sample lD Path

Unknown Sel11 11 C :U(cal ibur\Data\EDTA\BreweAS E L_Negative

Inst Method Proc Method Cal File Position lnjVol Level Sample Wt

C :Xcal ibu r\methods\EDTA_N eg_Swabs 11 5.0 0.000


U.UUU 0.000 1.000

Sample Name:

Comment:

, MAL, Yellow, d12 spiked

Study:

Client:

Laboratory:

Company:

Phone:


Unknown Sel12 12 C :V(calibur\Data\E DTA\B reweAS EL_Negative


C : U(cal ibu r\meth od s\EDTA_N eg_Swabs 12 5.0 r0.000I


O.UUU 0.000 1.000

to +*a( sa),

1001

;ilssl80-l

"-]ro-l

.u-l 1

8 60-.'l

ualzlvl 1uiz1:J4

m'lz= 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.s01 MSSel01

Time (mn)

nJz= 282.V2U.3F: - cESI SRM [email protected] [282.7U2U.251 MSSel01

tp aU( sat

NL:2.96E4rnlz=272.5-273.5 F: - cESI SRM [email protected] I?46.50-247.50,272.50-273.501 MSSel0l

DWaO A, \JaSC |, lJrt,y J'rNL: 1.08E4rniz= 299.5-300.5 F: - cESI SRM [email protected] I299.50-300.50.325.50-326.50t MSSel01

ESI SRM [email protected] [299.50.300.50.325s0-326.501 MS

ESI SRM [email protected] [31r5G312.501 MS

Time (min)

02112107 10:32:28

3.91 E4nlz=246.*247.5F.-cESI SRM [email protected] [246.50-247.50.272.s&273.501 MSSel02

1.29E3filz= 282.8-2U.3F:. - cESI SRM ms2303,[email protected] I282.7t284.2s1 MSSel02

[, v+

Time (min)(t,o)

Swab A, Case 2, Red

nr/z= 299.S300.5 F: - cESI SRM [email protected] I,oo qn_1nn 6n32s.50.326.501 MSSel02

nvz= 325.S326.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSSel02

m/z= 31'1.5-312.5 F:- cESI SRM [email protected] [311.50.312.501 MSSel02

Time (mrn)

, C:U(calibuA...\SEL-Neeafiv@!],/ 02112J07 1O:43:17

NL:1.92E4ilz=272.5-273.5F: - cESI SRM [email protected],50-273.501 MSSel03

Ir'lz=246.5-247.5Fi - cESI SRM ms2291 [email protected] [246.9-247.fi.272.50-273.501 MSSel03

nlz=282.8-28/..3F:. - cESI SRM ms2303:[email protected] [282.7$.284.2s1 MS

1 00-l

^^l"r-l

I

oc6

o

.E

10(

9:

8:

80

7t

70

4

55

40

30

Time (min)

Swab B, Case 2, Grey JAP

Tlme (min)

C : u{ca I i bu 4...\S e L-N e gaIv(\Se to1) 021207 10:54:09 Swab C, Case 3-1, Grey ,Jr/13

NL: 1.21 E4trl/z= 299.5-300.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSSel04

NL: 7.73E3r/z= 31 1.5-312.5 F: - cESI SRM [email protected] [311.50-312.501 MSSel04

NL: 1.34E4ttlz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50,272.5&273.501 MSSel04

rn/z= 325.$326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSel04

o

d

o

o

tr- u,l ilx

NL: 3.74E3mlz=282.8-2U.3 Fi - cESI SRM [email protected] [282.7s.2U.251 MSSel04

Time (min) Time (min)&4

C:XcalibuA...\SEL_Negativ{9eP 0212107 't 1:04:58 Swab C, Case 3-2, Red J I'P

10(

9l

9(

AI

8(

7l

7(

8etSs.

NL: 1.09E4ftUz= 272.$273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSel05

tt!z= 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSelos

.r/z= 282.8-28/'.3 F: - cESI SRM [email protected] [282.75-284.251 MS

NL: 5.04E3m/z= 299.$300,5 F: - cESI SRM msZ3,[email protected] I299.50-300.50,325.50-326.501 MSSel05

r/z:325.5-326.5 F: - cESI SRM ms23,[email protected] [299.50-300.50,325.50-326.501 MSSel05

r/z= 31 1.5-312.5 F: - cESI SRM ms2356,[email protected] [311.50-312.501 MSDEIUJ

E6

€o

6

10c

Yi

8t

Af

7,

7C

CL

45

40

30

f" qs


( s'"t)

C :Xca I ib q 4...\S e l-ru"S"tiu{@ 02/12/0711:15:48

NL;4.26E4nlz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSel06

1.88E4rnlz= 246.t247.5 F: - cESI SRM ms2291 [email protected] [246.fi-247.50.2725o-273.50i Ms

nlz= 282.8-28/.3 Fi - cESI SRM [email protected] [282.75-2A4.251 MSSel06

I

o

.Eo

100

93

90

80

70

65

60

55

45

40

t<

30

Time (min)

Swab C, Case 3-3, Grey :TOP

NL:1.20E4m/z= 299.5-300.5 F: - cESI SRM [email protected] I299.50.300.50,325.50.326.501 MSSel06

z,otE5rtz= 325.5-326.5 F: - cESI SRM [email protected] [[email protected],32s.50-326.501 MS

Time (min)

, C:Xcalibur\...tSEt-t tegativdsepZ) 02112107 11:26:37

NL:4.74E3$lz=272.$273.5Fi - cESI SRM [email protected] [246.50-247.il,272.s0-273.501 MsSel07

1.96E4nn-246.*247.5Fi -cESI SRM ms229120@1s,00 I246.fi-247.50.272.s0-273.50i MSSel07

'r'lz=282.8-2U.3F: - cESI SRM [email protected] [282.75-284.251 MSS€107

[y +,/a( tor)

Swab D, Case 34, Grey 10r

1 00-t

aq!*1*t

-. 1'-l70-J

L

oci

*.]sq

NL:7.88E3m/z= 299.5-300.5 F: - cESI SRM [email protected],325.50-326.501 MSSelo7

i2.23EgtrVz= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,32s.50-326.501 MsSel07

b.ZYEJntlz= 311.5-312.5 F: - cESI SRM [email protected] I31 1 .50-312.501 MSSel07

oc6

€o

Tlme (min) Time (min)

NL: '1.48E4

mlz= 272.5-?73.5 F: - cESI SRM [email protected] [246.50.247.50.272.50-273.501 MSSel08

C:D(calibuA...\SEL_NeOativQp)

100

90

02i1U07 11:37''28 Swab D, Case 4-1, Red -rbpNL: 1.85E4rn/z= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSel08

1.O7E4rolru-l

ro-i,lE0-l

75-]I

::.1"lI 60-]ol

nlF 246.*247.5 Fi - cESI SRM [email protected] [246.50-247.50,272.50-273.s01 MSSel08

nlz=282.E-2U.3 F: - cESI SRM [email protected] [282.75-284251 MSSel08

m/z= 325.$326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSelOS

NL:7.79E3rn/z= 311.F.312.5 F: - cESI SRM [email protected] [311.50-312.501 MSSelOS

o

3eo

'nme (min) 'nme (min)

, C:U(balibuA.,.rSel-rueOativ@

lool oft

'lls'l I

02112107 1 1 :48:16 Swab D, Case 5, Red wp

mlz= 272.1273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.s01 MSSel09

ff{z= 246.5-247 .5 F: - cESI SRM [email protected] [246.fi-247.50.272.s0-273.501 MSSel09

rtlz= 282.8-2U.3 F'. - cESI SRM [email protected] MSSel09

[* uu,( s")

o

dE

5e@IoE

rn/z= 325.5-326.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSSel09

ESI SRM [email protected] [311.50-312.501 MSSel09


, C:U(calibuA...\SEL-NeSativgi 02112107 11:59:08 Swab A. MAL, Yellow -J Dtt'

1 00tI*l

oni*l

att

1001

;;,u-l

I

ro-.1

tul

'o-l

s .o-]ol

A lAEA

rlz= 246.5-247 .5 F'. - cESI SRM [email protected] [246.50-247.fi,272.50-273.s01 MSSel l0

qvb

Time (min)

(2,)

NL: 9.55E3rn/z:299.$300.5 F: - cESI SRM [email protected] [299,50-300.50,325.50-326.501 MSSel10

z.vlEJrl/z= 325.$326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSel10

Time (min)

C :lXcalibu A...\S EL-NeOati{}p

7

NL: 7.28E3nrlz=272.*273.5F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSell'l

nlz=246.U24?.5F: - cESI SRM ms2291 [email protected] [246.fi-247.fi,272.50-273.s01 MSSelll

0?112107 12:10:01

:1.'llE6ntlz=282.6-28/..3F:- cESI SRM [email protected] [282.7r2U.251 MSSell'l

Swab A, MAL, Yellow, d12 spiked -JbP

1001

--l,"1qnJ--l

NL:2.06E3dz= 299.5-300.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSSell 1

rnlz= 325.5-326.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSSell l

:3.74E4

o

o

oo

miz= 3'l 1 .5-312.5 F: - cESI SRM [email protected] I311.50-312.5O1 MSSel11

80

70

{n,tq{"

Time (min)

(t,tTime (min)

C lXcalibur\...\SEL-NeSativeEP 0211A07 12'.20:51 Swab D, MAL, Yellow, 01z sptKeo Jv7

NL:3.25E3nr/z= 299.$300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSel12

3.78E3r/z= 325.$326.5 F: - cESI SRM [email protected].

ms2r5.00 I

299.50-300.50,325.50-326.s01 MsSell 2

1.03E4r/z= 31 1.$312.5 F: - cESI SRM [email protected] [311.50-312.501 MSSel12

rool

nl*l

NL: 5.96E3r:.lz=272.5-273.5 F: - cESI SRM [email protected] (

246.50-247.fi,272.sG273.s01 MSSel12

NLi 8.03E3trtlz= 246.*247.5F: - c1001

*-lo.-l*l80-l

'u-lrol*l

8 60-lg -. I

ESI SRM [email protected] [246.fi-247.&,272.s0-273.501 MSSelt2

mlF 282.8-2u.3F'. - cESI sRM [email protected] [282.7$284251 MSSell2

@

F

€o

.Eo

Time (min)

L.O.D.

{* qlb(:is)

Sample Name:

C nent:

Sequence---LoD_neg. sld [Open]

100 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LODOl C:XcalibuAData\EDTA\Brewer\LOD NeoatMe g: V\calibur\methods\EDTA Nec

Proc Method CalFile Position lnjVol ,evel Sample Wt Sample Vol ISTD Amt

1 5.0 u.000 0.000 0.000

Sample Name:

Comment:

100 ppm EDTA

r*****************

*********t**************t*************************************

Study:

Client:

Laboratory:

Company:

Phone:

fl+uu( stu)nano 1

ft>[r'\o1

Proc Method Cal File Position!

InjVol Level Sample Wt Sample Vol ISTD Amt

1 5.0 0.000 0.000 0.000

Sequence---LOD_neg.sld [Open]

Sample Name:

C nent:

100 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path Inst MethodUnknown LODO3 01 : U(calibu r\Data\EDTA\BreweALO D_Negative G:U(calibuAmethods\EDTA Nei

Proc Method CalFile Position njVol Level Sample Wt Sample Vol ISTD Amt5.0 0.000 0.000 0.000

*******i*+*t*********t**t************tt**r********

Sample Name:

Comment:

ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type l-rle Name Sample lD Path lnst Method

Unknown LOD04 02 C :U(calibu r\Data\EDTA\Brewer\tO[Negative C : Xca I ibu r\m etn oO s\EDTA_N e g

Proc Method Cal File Position InjVol Level Sample Wt Sample Vol ISTD Amt2 5.0 0.000 0.0u0 0.000

l********************************************i**********

5u a'/ bG,r)

-yit-vlvlo1

Sample Name:

c nent:

Sequence---LoD_neg. sld [Open]

50 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LODO5 02 C: U(calibu r\Data\EDTA\Brewer\LOD_Negative G: V(cal i bu r\method s\EDTA_Neg

Proc Method CalFile Position lnjVol Level Sample Wt Sample Vol ISTD Amt2 5.0 0.000 0.000 0.000

Sample Name:

Comment:

ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type ile Name Sample lD Path Inst Method

Unknown LODO6 02 C : Xcali bu r\Data\E DTA\Brewer\LO D_Negative C:Xcalibur\methods\EDTA Nec

Proc Method CalFile Position lnjVol Level Sample Wt Sample Vol ISTD Amt2 5.0 u.uuO 0.000

**#*****************t*******************t************t********t

5, 4,/ e3,s)

-OI0Y

"tlpl"1

"t. " ''

Sample Name:

c rent:

Sequence---LOD_neg. sld [Open]

25 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

f******i*******t*****i*************t********s******tr*t***************r*****************


Unknown LODOT 03 C : U(calibur\Data\EDTA\Brewer\LO D_N egative :v\caltbur\rnethods\EDTA Nec

Proc Method Cal File Position lnjVol Level Sample Wt Sample Vol ISTD Amt

3 5.0 u.000 0.000 0.000

Sample Name:

Study:

Client:

Laboratory:

Company:

Phone:

uample lype File Name Sample lD Path Inst Method

Unknown LoD08 ]03 C : U(cali bu r\Data\EDTA\BreweALO D_N egative C:Xcalibur\methods\EDTA Neo


3 5.U 0.000 rJ.u00 0.

- qq/o

(:^'^,\

7rVvl,'lc1

J '",'

Sample Name:

e rent:

Seq uence---LO D_neg. sld [Open]

25 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

Sample Name:

Comment:

ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

****************t************r**s**************************s*****t****t*****

Sample Type File Name Sample lD Path Inst MethodUnknown LODOg 03 C :Xcalibu AData\EDTA\B reweALOD_t',I eg ative C:U(calibuAmethods\E DTA Nec

Proc Method CalFile Position InjVol Level Sample Wt Sample Vol ISTD Amt.3 5.0 0.000 0.000 0.000

******t*********

Sample Type ile Name Sample lD Path Inst MethodUnknown LOD1O 04 C:U(calibu r\Data\E DTA\B reweAIOD_N egEtive U:\Xcatrbur\methods\EDTA Nec

Proc Method CalFile Position InjVol Level Sample Wt Sample Vol ISTD AmtAA 0.000 0.000 0.000

Quuuba)

ApU

Ylvl"1

-,

Sample Name:

C rent:

Sequence--LOD_neg. sld [Open]

13 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

********t*********************t**t**********t******s***t****************t********************t****iis***********t**********ffi********

Sample Name:

Comment:

13 ppm

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD11 04 C :U(calibuAData\EDTA\Brewer\LO D_Negative C:\)(calibur\methods\EDTA Neo

Proc Method CalFile Position njVol Level lSample WtI

Sample Vol ISTD Amt

4 5.0 0.000 0.000 0.000


Unknown LOD12 04 C :U(calibu AData\EDTA\BreweALO D-Negative C:U(calibur\methods\EDTA N

Proc Method CalFile Position lnjVol evel Sample Wt Samole Vol ISTD Amt

4 5.0 0.000 0.000 0.000

****t***********

{o q,/,-( zt,\

zfoJDY

)lru'\21

6 ppm EDTA

Seq uence---LOD_neg. sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:

********t*tf ******************************t********i*****f *r

Study:

Client

Laboratory:

Company:

Phone:

Sample Name:

r lent:

Sample Name:

Comment:

ppm EDTA

Sample Type File Name Sample lD Path lnst MethodUnknown LOD13 05 \/\Ldiluut \ua[a \tru I A\E'rewer\Luu_Nggatlv€ :v(calibur\methods\EDTA Nec

Proc Method Cal File Position lnjVol Level Sample Wt Sample Vol ISTD Amt5 5.0 0.000 0.000 0.000

Sample Type File Name Sample lD Path Inst MethodUnknown LOD14 05 u : \xcatrbu r\Data\EDTA\B reweALOD_Negative C:Xcalibur\methods\EDTA I'teo

Proc Method CalFile Position InjVol Level lSample WtI

Sample Vol ISTD Amtc 5.0 0.000 0.000 0.000

.***************l***************tt********s**i

6. uoo(sta)

Tr?-t'ltvlal

q .'",.,

Sample Name:

n Ytent:

Sequence---LOD_neg. sld [Open]

ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path Inst MethodUnknown LOD15 05 :U(calibuAData\E DTA\B rewer\LO D-Negative u:v(calibur\rnethods\EDTA Nec

Proc Method Cal File Position lnjVol Level Sample Wt Sample Vol ISTD Amt5 5.0 0.000 0.000 0.000

Q vva( t:z)

anT'Vl'v\o1

C :\)(calibur\...\LOD-NeOativ@$ 0U1?i07 12:41:10 100 ppm EDTA J"?

n/z= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSLod01

fitlz= 246.+247.5 Fi - cESI SRM [email protected] [246.50.247.50,272.5O.273.s01 MSLodol

NL: 1.94E4BVz= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSLodo1

o

o

o

o

NL:0tf'lz=282.8-2U.3Fi -cESI SRM [email protected] [2A2.75-2U.251 MSLod0'l

fl/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSLod0l

fime (min)

02l1aa7 12'.45'.27

ftill=272.1273.5F: - cESI SRM [email protected]

ms2r5.00 I

246.56247.fi,272.5e273.s01 MS

100 ppm EDTA'\eu

I

rn/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50.300.50,325.50-326.501 MSLod02

:5.26E4nlz= 246.5-247.5F: - cESI SRM [email protected] I246.50-247.50,272.s0.273.501 MSLod02

o

ooo

NL:4.66E3nlz=282.8-2U.3 F: - cESI SRM [email protected] [email protected] [282J2$284.251 MS

6u,/,

: E.16E3nlz= 311 .5-312.5 F: - cESI SRM [email protected] I31 1.50.312.501 MSLod02

Time (min)

(t-ts

NL:6.6585mlz= 272.5-273.5F: - cESI SRM [email protected] I246.50-247.50,272.50-273.501 MSLod03

0211207 12:49:20 100 ppm EDTA T,F

n/z= 299.5-300.5 F: - cESI SRM [email protected] [299.5G300.50.325.50-326.50} MSLod03

t*r--l

*-l*.]*-l7sJ

?o-l

"1,8 60l

NL:4.28E4rnlz= 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.s0-273.501 MSLod03

nlz=282.8-2U,3F:. cESI SRM [email protected] [282J3$284.251 MS

6rw

1001

^-l--lso-]

als0-l

"lro-1,l60-l

--l*.]50-J

ou-]I

oo-l

*-l

(a sc.

C:Xcalibur\...\LOD_Negati 02h207 12:53:15 50 ppm EDTA 'TPP

10(

8(

7l

7(

ba

Qar

NL:4.19E4ntlz=272.*273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.s01 MSLodOl

ESI SRM [email protected] [246.fi-247.50,272.s0-273.501 MSLod04

mlz=282.8-2U.3F: - cESI SRM [email protected] [282.75-2u.251 MSLod04

NL:2.32E4rnlz= 299.5-300.5 F: . cESI SRM [email protected],qo qo-?no qn

325.50-326.501 MSLod04

:3.31E3r/z= 325.$326.5 F: - cESI SRM [email protected] I299.50-300.50.325.50-326.501 MSLodOl

3,41E3r/z= 311.$312.5 F: - cESI SRM [email protected] [311.50-312.s0j MSLod04

I6

e@

-c

1.5Time (min)

E,v

C:l(calibur\...\LOD_Negativ

0.77

02fi407 12:57:07

NL:'1.77E3

'r'lz= 246.5-247 .5 F: - c

NL:1.34E4mlz=272.5-273.5 Fi - cESI SRM [email protected] [246.&-247.50,272.50-273.501 MSLod05

ESI SRM [email protected] [246.50-247.50,272.5C273.sO1 MSLod05

NL:0rnlz:- 282.V2U.3 F: - cESI SRM [email protected] [282.75-2u.251 MSLod05

IF

)€o

@oE

Time (min)

& vq,

50 ppm EDTA joP

r/z= 325.5-326.5 F: . cESI SRM [email protected] {299.50-300.50,325.50-326.501 MSLodO5

NL: 6.90E3rn/z=311.5-312.5 F:.cESI SRM [email protected] [311.50-312.501 MSLod05

Time (min)

C :U(ca libuA...\LOO-Nesativ6';b 0?J12107 01 :01:00

NL:4.54E5rtlz= 272.5-273.5 F: - cESI SRM [email protected],272.50-273.s01 MSLod06

ftlz=246.5-247.5 F: - cESI SRM msz29120@15,00 [246.50-247.fi.272.50.273.501 MSLod06

€-

50 ppm EDTA ')pt'

1 o0l

--l

^.1

7.54E3

o

o

€o

.Eo

nr/z= 325.$326.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.501 MSLod06

r/z= 311.5-312.5 F: - cESI SRM [email protected] [311.s0-312.501 MSLod06

10(

8:

EO

7C

6C

55

40

30

1.5nme (min)Time tminl

bD

C :U(calib ur\...\LO O-f.f "Orr'@ 0211A07 01:04:53 25 ppm EDTA

100-t

oJ*l-J

ESI SRM [email protected] [246.50-247.50,272.50-273.501 MS

NL:123E4

']/z= 246.5-247 .5 F: - c

ESI SRM [email protected] [248.50-247.50,272.50-273.501 MSLod07

NL: 1.63E4miz= 299.5.300.5 F: . cESI SRM [email protected],325.50-326.501 MSLod07

r/z= 325.5-326.5 F: - cESI SRM [email protected],325.50-326.50t MSLod07

NL:1.79E3nlz= 282.8-2U.3 F: - cESI SRM [email protected] I282.7$284.251 MSLod07

rvz= 311.5-312.5 F: . cESI SRM [email protected] MS

02J12107 01:08:47

NL:1.10E4r 1z.246,5-247.5F:-cESI SRM msz29'[email protected]@15.00 [246.50-247.50,272.s0-273.501 MS

25 ppm EDTA

NL:1.27E4nvz= 299.5-300.5 F: - cESI SRM [email protected] I299.50-300.50.325.50-326.50t MSLod08

1001

".]s5-l

8JI?l

?0-l

ari8 60--l

ffVz= 325.5-326.5 F: - cESI SRM [email protected] t299.50-300.50,-325.50-326.501 MSLod08

f,y 4+bGt)

0211A07 01:12:45 25 ppm EDTA

NL:2.44E4m/z= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.s0t MsLod09

NL:2.03E5nlz--272,5-273.5F: - cESI SRM ms2291,[email protected] [246.50-247.50.272.50-273.501 MSLod09

t00

90

AE.

E0.

65.

60.

55-

5U-

45-

40-

3$

30-

Io

e

!o

rn/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSLod09

4.73E3

[+ a(( tta

C :U(ca libur\...\LOD-NeSati{11E 0U12107 01:16:37 13 ppm EDTA atF0.77 NLi 4.42E4

'll/z= 272.5-273.5 F: - cESI SRM [email protected] I246.50-247.50,272.50-273.501 MSLod10

r'lz=246.+247.5F:. cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSLod10

NL: 0tnlz=282.8-2g.3 F: - cESI SRM [email protected] [282.752U.251 MSLod10

ood

:o

=

8.91E2m/z= 3'11.$312.5 F: . cESI SRM [email protected] [311.50-312.501 MS

f+ q((zst)

NL:2.'13E4m/z= 299.5-300.5 FESI SRM [email protected] I299.50-300.50,'325.50-326.50t MSLod'10

02112107 01:20:32

NL:6,86E4rniz=272.5-273.5 Fi - cESI SRM ms2291 [email protected] [246.50-247.50.272.50-273.s01 MS

:9.E7E3f,]lz=246.5-247.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.s01 MSLodl I

.tlz=282.8-2U.3 F'. - cESI SRM [email protected] [282.75-28/.251 MSLodt'l

od

o

@o

tr qq

( ts+

13 ppm EDTA Jtg

fEDTfjronl

1.00E4m/z= 325.5-326.5 F: . cESI SRM [email protected] [299.50.300.50.325.50-326.501 MSLodll

r r1trarvz= 3 l 1.5-31 2.5 F: - cESI SRM msz3s6,[email protected] I3'11.50-3'12.501 MSLodl 1

0?i1?i07 01:24:25 13 ppm EDTA

NL:8.62E4nlz=272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50.273.501 MSLod12

NL:2.45E3rfllz=282.*2U.3 Fi - cESI SRM [email protected] [282Js-2U.251 MS

qv

8f,

o

.go

NL: 1,76E4nr/z= 299.5-300.5 F: . cESI SRM [email protected] [299.50.300.50,325.50-326.501 MSLodl2

r/z= 325.S326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSLod12

r/z= 31 1.''312.5 F: - cESI SRM [email protected] [311.50-312.501 MSLod'12

Cv

1.5Time (min)

1.5 2.0Time (min)

:5.86E3rnlz=246.*247.5 F: - cESI SRM [email protected] [246.50-247.9,272.s0-273.501 MSLod12

( 3ss

02112107 01:28:18 6 ppm EDTA

r/z= 299.5-300.5 F: - cESI SRM ms2ms2

r5.00 [[email protected] [299.50-300.50,325.50-326.501 MSLod13

nvz= 325.5-326.5 F: - cESI SRM [email protected] I299.50-500.50,'325.50-326.50t MSLodl 3

m/z= 31 1.5-312.5 F: . cESI SRM [email protected] [311.50-312.50) MSLodl 3

1 00-l

^-l'ls0J

^-l

;;l?5-]

I

to-1

uuJ

q

0?/1?./07 01:32:10 6 ppm EDTA

NL:2.77E4nlz=272.$273.5 F: - cESI SRM [email protected] I246.50-247.50,272.50-273.50t MSLod'14

m/z= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSLodl4

1001

"-ls0-1

n<--l*lro-l

75-..1

7o-.1I*l

I 60-]-l

mlz= 246.*247.5 F: - cESI SRM [email protected] [246.50.247.50.272.50-273.50t MSLod 14

NL:2.75E3r/z= 325.S.326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.s01 MSLod14

1.66E3(r|F282.8-2U.3F: - cESI SRM [email protected] [282-752U.251 MSLod14

tr.+,1,( )s't

l'lme (min)

C:U(calibur\...\LOD 0211207 01:36:03

,::::l

NL: 3.67E4nlz=272.5-273.5Fl- cESI SRM [email protected] [246.50.247.50,272.5&.273.501 MSLod15

&-,/w

o

6

€o

( 338

6 ppm EDTA JhPNL:5.92E3rvz= 299.5-300.5 F: - cESI SRM [email protected] [299.50.300.50.325.s0-U6.501 MsLodl 5

: 4.80E3rvz= 325.S326.5 F: . cESI SRM [email protected] MSLodl5

NL:4.72E3trVz= 31 1.t312.5 F: - cESI SRM [email protected] [311.50-312.501 MSLod15

0.53

A

/\

tl

Seq uence--LOD2_neg. sld [Open]

Sample Name:

C--nent:3 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD16 05 C:Xcalibur\Data\EDTA\Brewer\LOD Neoative G:Xcalibur\methods\EDTA Nec


o b.u 0.000 0.000 0.000

Sample Name:

Comment:

ppm

Study:

Client:

Laboratory:

Company:

Phone:

tH*****s******t*it**********************t*****************i*********************************t***ff**********

€r q(u( 3)q)page 1

7*Vp\r,\'1


o 5.0 0.000 0.000 u.00u

Sequence--LOD2_neg. sld [Open]

Sample Name:

C^nment:

3 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

***********t**************t***********************************************i*t*+*********i*****t**************t******************************r**

Sample Name: .6 ppm EDTA

Comment: Study:

Client:

Laboratory:

Company:

Phone:

{n rl,lu( l+r)

page 2

5rl1Pto1

Proc Method GalFile Position InjVol Level Sample Wt Sample Vol ISTD Amto 5.0 0.000 u.000 0.000

Sample Type File Name Sample lD Path Inst MethodUnknown LOD19 05 :\Xcall bur\Data\E DTA\Brewer\LO D_Negative :\Xcallbur\methods\EDTA Nec

Proc Method Cal File Position InjVol Level Sample Wt Sample Vol IISTD Amr7 5.0 0.000 0.000 0.000

-

Sequence--LOD2_neg. sld [Open]

Sample Name:

C'-"nent:1.6 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Sample lD Path Method

Unknown LOD2O 05 :Xcalibu AData\EDTA\B reweALO D_Negative C:U(calibuAmethods\EDTA Neo

Proc Method Cal File Position lnjVol Level Sample Wt Sample Vol ISTD Amt.,t b.0 rJ.{J00 0.000 0.000

*******************s***i*******************i*************t*****************

Sample Name:

Comment:

1.6 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LoD21 105

C :\)(cali bu r\Data\EDTA\Brewer\LO D_N eg ative C:Xcalibur\methods\EDTA Neq


7 5.0 0.000 0.000 U.UUU

arV'Lltv\'ta

ht- VVb,/- \()ar\nana ? '/

02112107 01;46:39

1001

ru-l

*.1

851

*.]?l7q.*l

I 60-l

r]/z=272.1273.5Fi - cESI SRM ms2291 [email protected] [246.50-247.50,272.s0r73.501 Ms

{*a4

NL:0fil/z= 299.5-300.5 F: - cESI SRM [email protected] I299.50.300.50,-32s.50-326.501 MSLod16

325.5-326.5 F: - cESI SRM [email protected] r299.50-5oo.so.'325.s0-326.501 MS

NL: 1.83E3

'n/z= 246.1247 .5 F: - cESI SRM [email protected],272.50273.501 MS

filz= 282.8-2U.3F.. - cESI SRM [email protected] I282.75-2U.251 MSLod'16

r00l

ru-J

*-l8q8o-l

tr-l

'o-l6l60-]

-- |

"rlroloul

oo'1

,.]

G4j

' C:U(calibuA...\LOD 02l1VO7 01:50:58 3 ppm EDTA

NL:3.59E3nvz= 299.5-300.5 F: - cESI SRM [email protected] MSLod17

nlz= 246.$247 .5 F: - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MSLodl 7

o

o

-g

€o'/'lU

t7]lz= 282.8-2U.3 F: - cESI SRM [email protected] [282.7$284.251 MSLodlT

( t+)

C:XcalibuA...\LOD 0?J12107 01:54:50

NL: O

nlz= 272.5-273.5 F: . cESI SRM [email protected] [246.50-247.50.272.50-273.501 MSLod18

1.90E3r!z= 246.5-247.5 F: - cESI SRM [email protected] [246.&-247.50,272.50-273.501 MSLod'l I

3 ppm EDTA

o

oo

tn'/4b( z+'\

0A12107 01:58:43 1.F ppm EDTA

NL: 1.23E3m/z= 299.5-300.5 Fi - cESI SRM ms2344,[email protected],325.50-326.501 MSLodl 9

nlz= 246.*247 .5 Ft - cESI SRM [email protected] I246.5G247.50,272.50.273.s01 MSlod19

NL: O

n{z=282.V284.37: - cESI SRM [email protected] [282.7$.284251 MSLod'19

o

E

3.50E3

: 1 .35E3r/z= 31 1.5-312.5 F: - cESI SRM [email protected] [311.50-312.50j MSLod'19

, -dl,+DTFfi?A0.0 0.s 1.0 1:5 2.0 2.5 3.0

Lr q"(

rn/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSLod19

Time (mrn)Time (min)

( *s)

C:U(calibur\...\LOD_ 02112107 02:02:36

NL: 5.20E3.r/z= 272,5-273.5 F: - c

'ESl SRM [email protected] [' 246.50-247.50,272.50-273.501 MSLod20

.r.lz=2465-247.5 Fi - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MSLod20

nlz= 282.8-2a43 F'. - cESI SRM [email protected] I282.75-284251 MSLod20

1.6 ppm EDTA-l-oF

100-l

-"1-

NL: 1.98E3nriz= 299.5-300.5 F: - cESI SRM [email protected] I299.5C300.50,325.s0-326.501 MSLod20

m/z= 325.+326.5 F: - cESI SRM [email protected] {299.50-300.50,325.50-326.501 MSLod20

R

du

eo

-s!@

fn qva

( z+)Tlme (min) Trme (min)

RT:03d- 3o-5

100-l

ss-]I

'n-l

100-

v5-

90-

85-

80-

75-

60-

5J-

s-45-

40-

35-

30-

' C :Xca I ibu r\...tt-O O-N.g"tir6f;2l

0.77

0A1UO7 02:06:29 1.6 ppm EDTA 'f rpP

NL: 2.81 E3rtlz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSLod21

nJz= ?46.5-247.5 F: - EESI SRM ms2291 [email protected] [246.50-247.50,272.50-273.501 MSLod2l

fi1lz=282.8-2U3 F: - cESI SRM [email protected] [282.75-2U.251 M8Lod2l

@

6

o

o

rn/z= 299.$300.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSLod21

rvz= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50.326.501 MSLod21

rrz: 31 1 .5-3'12.5 F: - cESI SRM [email protected] [311,5S312.501 MS

{* aqG

{Sequence--LOD_pos. sld [Open]

Sample Name:

C- rent:

100 ppm

Study:

Client:

Laboratory:

Company:

Phone:

Sample Name:

Comment:

100 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

t**********i*************t*******i****************tf****t***t********t*t*****t*#**************tl

{rc (,t c'( vt)

oaqe 1


Unknown LODOl 1 C :Xcalibur\Data\EDTA\Brewer\LOD Positive :Xcalibur\methods\EDTA Pos

Proc Method CalFile Position nJvol Level Samole Wt Sample Vol ISTD Amt

1 5.0 0.000 0.000 0.000

Sample Type ile Name Sample lD Path lnst Method

Unknown LODO2 01 C:U(calibur\Data\EDTA\Brewer\LOD Positive C:U(calibur\methods\EDTA Pos


1 5.0 0.000 0.000 0.000

ft'>lr-1"'1

Sample Name:

C- '.nent:

Seq uence---LoD_pos. sld [OpenJ

100 ppm EDT

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Samole lD Path Inst MethodUnknown LODO3 01 C:Xcalibur\Data\EDTffi C:Xcalibur\methods\EDTA pos

Proc Method CalFile Position InjVol Level Sample Wt Sample Vol ISTD Amt1 5.0 0.000 0.000 0.000

Sample Name:

Comment:

ppm ED

******ti*****************i********t******t***t*********************

****t*******************************t*************r******

Study:

Client:

Laboratory:

Company:

Phone:

{r avu(t+';

naoe 2

:Tstlvi."t

Proc Method CalFile Position InjVol Level Sample Wt Sample Vol Amt2 5.0 0.000 0.000 0.000

Sample Name: rl(- nent Study:

Client:

Laboratory:

Company:

Phone:

***t*t***********************************************i*t************************t***********************t**************************t******l**t*

Sample Name:

Comment:

ppm EDT

Study:

Client:

Laboratory:

Company:

Phone:

**8**t******************t***************************************************************#***********i*********i*******t**r*************i***

Seq uence---LO D_pos. sld [Open]

[y +qb( zs')

JOF

Llttlc 7

C:Xcalibur\metnoOs\eDTR

Sample Name:

C nent:

Sequence---LOD_pos. sld [Open]

25 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LODOT 03 C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:U(calibur\methods\EDTA Pos


3 5.0 0.000 0.000 0.000

*******tl*************ii*******ff **f *********tr*******t

Sample Name:

Comment:

25 ppm

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LODOS )4 C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:Xcalibur\methods\EDTA Pos

Proc Method Cal File lPositionI

InjVol Level Sample Wt Sample Vol ISTD Amt

3 5.0 0.000 0.000 0.000

t***t**t*********************l******

fr qqc'

^^l^t^'n

ArF'ultl"'7

Sample Name:

C- 'nent:

Seq uence--LOD_pos. sld [Open]

25 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LODOg 03 C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:U(calibur\methods\EDTA Pos

Proc Method Cal File Position InjVol Level Sample Wt Sample Vol ISTD Amt3 5.0 0.000 0.000 0,000

Sample Name:

Comment:

13 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown oD10 04 C:Xcalibu r\Data\EDTA\Brewer\LOD Positive C:U(calibur\methods\EDTA Pos


4 5.0 0.000 0.000 0.000

*************t

fo'/u,(st^)

oaoe 5

Jb!uf vf "t

Sample Name:

C- '.nent:

Sequence--LOD_pos. sld [Open]

13 ppm

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD11 04 C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:Xcalibur\methods\EDTA Pos

Proc Method CalFile Position InjVol Level Sample Wt Samole Vol ISTD Amt

4 5.0 0.000 0.000 0.000

**t*****t*******************i**************t***********t**t*******

Sample Name:

Comment:

13 ppm E

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD12 04 C:XcalibuAData\EDTA\Brewer\LOD Positive C:Xcalibur\methods\EDTA Pos

Proc Method Cal File iPosition InjVol Level Sample Wt Sample Vol ISTD Amt

4 5.0 0.000 0.000 0.000

**********t*t********************************i***********

tn u+o( zs)

nana A

JrfLlvl"1

Sample Name:

C rent:


6 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD13 05 :U(calibuAData\EDTA\BreweALOD Positive C :U(calibur\methods\EDTA Pos


5 5.0 0.000 0.000 0.000

***t*****************

Sample Name:

Comment:

6 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD14 05 C:\)(calibur\Data\EDTA\BreweALOD Positive C :U(calibur\methods\EDTA Pos


5 5.0 0.000 0.000 0.000

***********************************t*t******l*******************t**************************

{'* ou o( zs+)

aaaa'7

-,nJ DI'II'L ItLl2 7

Sample Name:

c nent:

Sequence---LoD_pos. sld [Open]

6 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD15 05 C:U(calibuAData\EDTA\BreweALOD Positive C:U(calibuAmethods\EDTA Pos


5 5.0 0.000 0.000 0.000

Sample Name:

Comment:

3 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD16 UO u : \xcal tbu r\uata\tsLJ I A\H rewer\Lu u Postttve C:U(calibur\methods\EDTA Pos

Proc Method Cal File Position njVol Level Sample Wt Sample Vol ISTD Amt

5.0 0.000 0.000 0.000

fr. uuo( zs) JbF

t lwbt

Sample Name:

C -nent:

Sequence--LOD_pos. sld [Open]

ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD17 06 C:U(calibur\Data\EDTA\Brewer\LOD Positive C:U(calibur\methods\EDTA Pos


c 5.0 0.000 0.000 0.000

*****************t*****s*tr*t*********i******************tt**t**t*i********t**********s*******t***r*******ti*********t***********r***********

Sample Name:

Comment:

3 ppm EDTA

sampre rype File Narne Sample lD Path lnst Method

Unknown LOD18 06 C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:Xcalibur\methods\EDTA Pos


5.0 0.uuu 0.000 0.000

f'r aqb( es)

nana O

'Jrf

rlvl"t

Sample Na

(- nent:


1.6 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

Study:

Client:

Laboratory:

Company:

Phone:


Unknown LOD19 07 C:UKcalibur\Data\EDTA\BreweALOD Positive C:U(calibur\methods\EDTA Pos


7 5.0 0.000 0.000 0.000

Sample Name:

Comment:

1.6 ppm


Unknown LOD2O 07 C:U(calibur\Data\EDTA\Brewer\LOD Positive C:\)(calibur\methods\EDTA Pos

Proc Method Cal File Position njVol Level Sample Wt Sample Vol ISTD Amt

7 5.0 0.000 0.000 10.000

fr'/'/('( zst) {bF

,lrr-lo1

Sample Name:

C -rent:

Sequence---LOD_pos.sld [Open]

.6 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:

{r 4ab( zst)

Sample Type File Name lSample lDI

Path lnst Method

Unknown LOD21 07 C:U(calibur\Data\EDTA\BreweALOD Positive C:Xcalibur\methods\EDTA Pos


7 5.0 0.000 0.000 0.000

tr,11'l ' 1

C:\)(calibuA...\LOD_Positive\Lod01.

-

02112107 02:43:57

1001

'-t

NL:4.04E5rVz= 159.5-160.5F: + c ESI Full [email protected] MSLod01

F: + c ESI Full [email protected] [r25.00-315.001 MsLod0l

1001

vvl

ro-]I*l

nnl*l75-..1

I

701

^-lIfl ao-.1

I

: 5.47E5TIC MS Lod01

(-{( ts'i

100 ppm EDTA

-

t-ltF101#60 RT: O.81 AV: 1 NL:4.55E5+ c ESI Full ms2 [email protected] [ 125.00-315.00]

C :U(calibur\...\LOD_Positiveld02- 02112/07 02:47:51

rol*I

NL:4.16E5nYz= 159.5.160.5F: + c ESI Full [email protected] MSLod02

NL:5.06E5TIC MS Lod02

IG2.6€

Time (min)

2052.80

t" 'l( eL,i

100 ppm EDTA

+ c ESI Full ms2 293.00@'15.00 [125.00-315.00]

1001

ru-l

*-lAE.]*t'l'l'l6l

o ^^l,1

,ol

'u-]

'o-]*-l

'l7ff..]uu-]

60-l

*.]5o-l z

I 0.0845_1 t

4/1il'lll

C:\)(calibuA...\LOD_Positive\Lod04

8076 1.06

02l1AO7 02:55:29

NL:3.76E4rniz= 159.$160.5F: + c ESI Full [email protected] [125.0G315.001 MSLod04

: l.zEEiTIC MS Lod04

oo6

oo=do

(o uu,( zuz

50 oom EDTA

tu4*i6 Kt: u./6 Av:1 NL: b.ZUE4+ c ESI Full ms2 [email protected] [125.00-315.00]

l

I

I

I

C:U(calibuA...\LOD_Positive\Lod05 02112107 02:59:15

NL:8.6'1E4rn/z= 159.$160.5F: + c ESI Full [email protected] I12s.00.315.001 MsLod05

65-

N-

45-

40-

zb

20-

't5-

10-

trtlz- 246.5-247 .5F: + c ESI Full [email protected] I't25.00-3'15.001 MSLMUS

t,a

: 1.00E4

(tat

+ c ESI Full msz [email protected] [ 125.00-315.00]

C :U(calibuA...\LOD_Positive\Lod06 0211i/07 03:03:06

1OGr

^-l'lNL:5.82E4rn/z= 159.5-160.5F: + c ESI Full [email protected] [125.00-3'15.001 MsLod06

,ol

*-lru-]ao!*ttr-l

1lo"-'l,'1

F: + c ESI Full [email protected] [125.00-315.001 MSLod06

1.42E4


o

oofE

o

oox,

{oqu(

50 ppm EDTAa---

1 NL:+ c ESI Fullhs2 [email protected] [125.00-315.001

160

RT: 0.00

1 00-l

*l

C :\)(calibu r\...\LOD_Positive\LodO7-

43 0.71

0.85

02112107 03:06:59

9.40E3nlz= 246.U247.5F: + c ESI Full [email protected] [125.00-315.001 MSLodo7

NL: 1.99E5TIC MS Lod07

ta0.33

1.5Time {min)

25 ppm EDTA ,

: + c ESI Full ms2 [email protected] [ 125.00-315.001

oo6!

o.zoo

C :U(calibuA...\LOD_Positive\Lod09, 0212/07 03:14:36

'ol*lNL: 1,69E4rn/z= 159.$160.5F: i c ESI Full [email protected] [12s.0G315.001 MSLod09

4.42E3

1001

ru-]

*-l,u-]FAJ*l75-i

to-]

^J--tP 'nl

tr'lz= 246.5-247 .5F: + c ESI Full [email protected] [12s.00-315.001 Ms

oo6

4o6E

-NL:2.18E5j.!2, rrc us r-oaos

fo,l,l o

luvRiz Kt: u.64 Av: I NL: 2.ZtE4+ c ESI Full ms2 [email protected] [ 125.00-315.00]

2.01E3

1001

,5-l

*-18s-l

'o-ltu-l

7o--l

.'- ]

rnlz= 246.*247 .5F: i c ESI Full [email protected] [125.00-3't5.001 MSLod08

to q+

(r"l


C:\)(calibuA...\LOD_Positive\Lod 1 0

5 qatra

,:l"l*J*lrnJ--lzs--l

I

toJ

*lI

rilz= 246.*247 .5F: i c ESI Full [email protected]'15.001 MsLodl 0

{,^t +'l t"(tus)

od10*r61 RT: 0.83 AV: 1 NL: 3.45E4: + c ESI Full ms2 [email protected] [ 125.00-315.00]

C :l(calibur\...\LOD_Positive\Lod 1 1 0A1ZO7 03:22:11

t*-]*l*.1*.180-l

7s-l

,0-l

" ':-]

NL: 1.89E4m/F 159.$160.5F: + c ESI Full [email protected] [125.00.315.001 MSLodl 1

NF246.5-247.5F: + c 551 Pr1 t"[email protected] [125.0C315.001 MSLodi 1

[+ aau( 2,,,q\

: + c ESI Fult ms2 [email protected] [ 125.00-315.00J

C:\)(calibuA...\LOD Positive\Lod12 0?/12107 03:26:02

1 00-lI

s5-1

""-lAqJ--tnnJ*lru-l

70-JI

ai-J--lP -l

nlz= 246.$247.5F: + c ESI Full [email protected] I125.00-315.00t MSLod12

f,r 4,tb

ar i4

: z.ocE3TIC MS Lodl2

13 ppm EDTA

-

0d1?#61 Rl:0.E3 AV:1 NL:2.42E4: + c ESI Full ms2 [email protected] [ 125.00-315.001

Eo

o66tr

C:XcalibuA...\LOD Positive\Lod 1 3

64or. 0.87

02112107 03:29:50

NL:1.03E4n/z= 159.$160.5F: + c ESI Full [email protected] l125.00-315.001 MsLod13

227E3n|F246.1247.5F: + c E6l Full [email protected] |125.00.315.001 MSLod13


€t.3

6 ppm EDTA

l'13#63 t{l: u.65 AV: I NL: J.zbE4+ c ESI Full ms2 [email protected] [125.00-315.001

C :U(calibur\...\LOD_Positive\Lod 1 4 02112107 03:33:39

NL; 1.29E4n/z= 159.F160.5F: + c ESI Full [email protected] MSLod14

1001

;*.]*-l

'lto'1

--lo -. 1-t

rnlz= 246.5-247.5F: + c ESI Full [email protected] MSLod14

:2.46E5TIC MS Lod 14

tn,tu,( tt,t

0?/1U07 03:37:26

NL:'1.91E4rvz= 15S.5-160.5F: + c ESI Full [email protected] [125.00-315.001 MSLod15

ty aau

':l"l*l*lrol

'l7H

"-l. ^^lc -t

( ztz


C:U(calibur\...\LOD_Positive\Lod 1 6

100-rI

--l

0?J12107 03:41:16

NL: 2.31 E4nvz= 'l 59.5-1 60.5F: + c ESI Fult [email protected] [125.00-315.001 MSLodl 6

fttlz= 246,5-247.5F: + c ESI Full [email protected] [125.00-315.001 MSLod16

ooo

f

o

.co

2.27E5TIC MS Lodl6

t* qqo

( n+)

3 ppm EDTA

-

Full ms2 [email protected] [ 125.00-315.00]

C:U(calibuA...\LOD Positive\Lod 1 7 02112/07 03:45:05

2.78 rnlz= 246.5-247.5I F: + c ESI Full ms2

[email protected] [125.00-315.001 MS

oo6€foo6EE,

2.01E5TIC MS Lod17

fr qo

1662.26

( tts

3 ppm EDTA

--+ c ESt Fuil ms2 [email protected] [ 125.00-315.00]

263

I

I

I

C :U(calibuA...\LOD_Positive\Lod 1 8 041U07 03:48:52

':iNL:7.78E3rnlz= 159.5-'160.5F: + c ESI Full [email protected] [125.00-315.001 MSLodlS

: l.l3E31001

rulel*l*-lru-l

to-]

6l" -n-l

ft/z=246.5-247.5F: r c ESI Full [email protected] [125.00-315.001 MSLodl I

'NL:229E5

TIC MS Lod18

ooE!aooo6E.

{r,1,1( z'tu

3 ppm EDTA


MATRIX

fo vqu( ztt)

.0

Sample Name:

n -ment:

Seq uence---MATRIX_pos. sld [O pen]

("50 ppm")

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXOl I C :\Xcalibu r\Data\E DTA\BreweAMAT Positive




0.000 0.000 1.000

Sample Name:

Comment:

atrix

Study:

Client:

'l-aboratory:

Company:

Phone:


Unknown MATRIXOz 02 C:Xcalibur\Data\EDTA\Brewer\MAT Positive

lnst Method Proc Method CalFile Position InjVol Level lSample Wt



0.000 0.000 1.000

************i

f,* uo,;I rts)

nana 'l

-..,tr(.Llpl.1

Sample Name:

C--rment:

Sequence---MATRIX_pos. sld [Open]

Matrix 8 ("50 ppm")

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXO3 03 :XcalibuAData\EDTA\Brewer\MAT Positive

Inst Method Proc Method CalFile Position InjVol Level Sample Wt

C:U(calibur\methods\EDTA Pos Swabs 8 5.U 0.000


0.000 0.000 1.000

*ff****t*****

Sample Name:

Comment:

9 ("50 ppm

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXO4 04 C:U(calibur\Data\EDTA\Brewer\MAT Positive

lnst Method Proc Method CalFile Position InjVol Level lSample Wt

C:XcalibuAmethods\EDTA Pos I 5.0 0.000


0.000 0.000 1.000

*****************************t***********************t*************t***********************t*********t**************************************

/'L4(

+tlb)'11\

{q0r lrr \:1

nana )

Sample Name:

f---rment:

Seq uence---MATRIX_pos, sld [Open]

Makix 10 ("50 ppm")

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXOS 05 C:U(calibuAData\EDTA\Brewer\MAT Positive

Inst Method Proc Method CalFile Position njVol Level Sample WtC:Xcalibur\methods\EDTA Pos Swabs 10 5.0 0.000


0.000 0.000 1.000

Sample Name:

Comment:

50 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXO6 06 C:U(calibuAData\EDTA\Brewer\MAT Positive

Inst Method iProc Method


0.000 0.000 1.000

f* *of-( zs)

nana ?

{rPr- lrr-\o1

Sequence--MATRIX_pos. sld [Open]

Sample Name:

C^"rment:

ppm

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXOT 06 C:XcalibuAData\EDTA\Brewer\MAT Positive

lnst Method Proc Method Cal File Position lnjVol Level Sample Wt



0.000 0.000 1.000

****t**t*****t**********+*l*s*t***tt*********************t**

Sample Name:

Comment:

50 ppm EDTA

Study:

Client .

Laboratory:

Company:

Phone:


Unknown MATRIXOS UO C:U(calibur\Data\EDTA\BreweAMAT Positive


C:U(calibur\methods\EDTA Pos Swabs 12 5.0 0.000


0.000 0.000 1.000

****t***t********s******t**********************************t***********

tu +Vt"( +s)

oaoe 4

4"0Lf t- i"e


Sample Name:

/^-rment Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXOg 06 C :U(cal ibu r\Data\EDTA\Brewer\MAT Positive

lnst Method Proc Method CalFile Position lnjVol Level Sample Wt

C:Xcalibur\methods\EDTA Pos Swabs 12 c.tJ 0.000


0.000 0.000 1.000

Sample Name:

Gomment:

50 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


unKnown MATRIXlO 12 ;:u(calrDur\Data\tsu I A\Hrewer\MA I Posttve




0.000 0.000 1.000

*f ***********t*******

{+ a+ulrse)

naoe 5

T'rP1lt'\'r

Sample Name:

' .ment:

Seq uence---MATR lX_pos. sld [Open]

Matrix 3 ("500 ppm")

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIX13 03 C :U(calibu r\Data\EDTA\Brewer\MAT Positive

Inst Method Proc Method Cal File Position njVol Level Sample Wt

C:U(calibur\methods\EDTA Pos Swabs 3 5.0 U.UUO


0.000 0.000 I.UUU

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXl4 o4 C:XcalibuAData\EDTA\Brewer\MAT Positive

Inst Method Proc Method CalFile Position lnjVol Level Samole Wt

:Xcalibur\methods\EDTA Pos Swabs 4 5.0 0.000


0.000 0.000 1.000

€* qqo(38,

aaaa 7

4ott\r'lJ

Sample Name:

c- rment:

Seq uen ce---MATR|X_pos. sld [Open]

Matrix 5 ("500 ppm:')

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXlS 06 C:Xcalibur\Data\EDTA\Brewer\MAT Positive

lnst Method Proc Method Cal File Position InjVol Level Samole Wt



0.000 0.000 1.000

f ********************t*

Sample Name:

Comment:

ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXl6 06 C:XcalibuAData\EDTA\BreweAMAT Positive

lnst Method Proc Method Cal File Position InjVol Level iSamole WtI

u:\xcaltbunmetnods\EDIA Pos swabs 11 5.0 0.000


0.000 0.000 1.000

V+to( g?D

5"0

r- \rr'to'1n:nc A

Sample Name:

c-rment:


500 ppm

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXlT 06 C:U(calibur\Data\EDTA\Brewer\MAT Positive




0.000 0.000 1.000

*******i*********

Sample Name:

Comment:

500 ppm

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXlS Ub C:U(calibur\Data\EDTA\BreweAMAT Positive

lnst Method Proc Method Cal File Position lnjVol Level Samole WtI



0.000 0.000 1.000

tr +w-( tss)

naoe 9

1n0 | ,4-t ^\.lt.l \\ b\r\

:"Sample Name:

c'rment:

Seq uence---MATR lX_pos. sld [Open]

ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIXl9 06 C:U(calibur\Data\EDTA\BreweAMAT Positive

Inst Method Proc Method CalFile Position lnjVol Level Sample Wt

C:Xcalibur\methods\EDTA Pos Swabs 11 5.0 U.UUU

Samole Vol ISTD Amt DilFactor

0.0u0 U.OOU r.000

Sample Name:

Comment:

500 ppm EDTA

Study:

Client:

Laboratory:

Company:

Phone:


Unknown MATRIX2O 06 C:U(calibur\Data\EDTA\Brewer\MAT Positive




0.000 0.000 1.000

{* v+uI 3 8/">

nana'lO

')ii"r^

Sequence--MATRIX_pos. sld [Open]"-Sample Name:

f- -ment:

Matrix 1

Study:

Client:

Laboratory:

Company:

Phone:


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Matrix 2

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C :D(ca libur\...\MAT_Positive\Matrix02 02112107 04:16:49

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NL:9.90E5rdz= 159.5-160.5 F:+ c ESI Full [email protected]'t5.001 MSMatnxo2

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Sample Type File Narne Sample lD Path

Unknown MATRIXOl 1 C :Xcalibur\Data\EDTA\BreweAMAT_Negative


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0.000 0.000 1.000

********i********t***ttr******tr***t*tt*****t************t*****a***t**i**************************r***********r**#******r********t*****

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Comment:

ix 9 ("50 ppm")

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Sample Type File Name Sample lD lPathUnknown MATRIXO4 U+ r./ : \Acat t0ur\uata\ts D t RtBrewer\MAT_Negative

Inst Method Proc Method uar rile PosIton InjVol Level Sample Wtrrsg_owaus 9 5.0 0.000


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Inst Method Proc Method CalFile Position nJvol Level Sample Wtu : \xcaltbu r\methods\EDTA_Neg_Swabs 10 5.0 0.000


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****it******************ts********i******l***********************************r******s**********

Sample Name: 50 ppm EDTA

Comment: Study:

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Unknown MATRIXO6 06 u: xcat ibu r\Data\EDTA\Brewer\MAT_Negative

Inst Method Proc Method Cal File Posrtron InjVol Level Sample WtC:U(calibur\methods\EDTA_Neg_SweG 12 5.0 0.000


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C-'-'ment:

Seq uence---MATR|X_neg. sld [Open]

50 ppm EDTA

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Unknown MATRIXOT 06 V(calibu r\Data\EDTA\BreweAMAT_Negatlve

Inst Method Proc Method CalFile Position InjVol Level Sample WtU : \Xcal tbu r\methods\EDTA_N eg_Swabs 12 5.0 0.000


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Sample Name:

Comment:

***********t******************t*****r*******t******tt*t**tt****l*t*****i*****t**+********S*t*****************

50 ppm

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Unknown MAIRIXOE i06 C :U(calibur\Data\EDTA\BrewenUAt_Negative

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T'-lnjVol Level Sample Wt

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Sequence--MATRIX_neg. sld [Open]

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l^ .ment:50 ppm EDTA

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Laboratory:

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Sample Type ile Name Sample lD Path

Unknown MATRIXO9 06 U : \Xcalibu r\Data\EDTA\Brewer\MAT_Negative

Inst Method Proc Method CalFile Position InjVol Level lSample WtG : xcali bu r\methods\E DTA_Neg_Swabs 12 5.0 0.000


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Sample Name:

Comment:

*t*********t************************************************t***********i****i*******i********t*t********

50 ppm EDTA

Study:

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Unknown MATRIXlO 12 C :U(cal ibur\Data\EDTA\Brewer\MAT_Negative

Inst Method Proc Method Cal File PositionI

InjVol Level Samole WtC :U(cal ibur\methods\EDTA_Neg_Swabs 112 5.0


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Comment:

Matrix ppm")

Study:

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Unknown MATRIX12 02 C:U(calibu r\Data\E DTA\B rewer\MAT_N egative

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Seq uence---MATR tX_neg. std [Open]

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Comment: Study:

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Sequence---MATRtX_neg. sld [OpenJ/

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Client:

Laboratory:

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sample Type File Name Samole lD Path

Unknown MATRIXl5 06 u:\ canDur\lJata\EDTA\Brewer\MAT-Negative


0.000 0.000 1.000

Sample Name:

Comment:

********t***************i*****t*t*************st**t******t***********ra************tr***

500 ppm EDTA

Study:

Client:

Laboratory:

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0.000 0.000 1.tJ00

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Seq uence---MATR lX_neg. sld [OpenJ

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0.000 0.000 1.u00

ffi*iff#s******#****lt*********i***ft*t*********a************t*ffi****t********t***********

Sample Name:

Comment:

ppm EDT,

Study:

Client:

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Sample Type Ftle Name Sample lD Path

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Sample Name:

Comment:

500 ppm EDTA

Study:

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RT:1.04AA:493664 NL: 2.93E4

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RT:0.92MA:164222

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M:70?4 NL: 4.91 E3m/z= 31 1.5.312.5 F: - cESI SRM [email protected] [311.50-312.501 MSMatrir03

NL:2.1184rTYz= 299.5-300.5 F: - cESI SRM [email protected] MSMatrix03

ttlz= 282 .8-294 .3 F i - cESI SRM [email protected] I282.7r2U.251 MSMatrixo3

{^t++t,

C :U(calibur\...\MAT_Negative\Matrix04

RT:0.93M:'18721

NL: 3.72E3rtlz=272.5-273.5F: - cESI SRM [email protected] I246.50-247.50.'272.s0-273.50i MSMatfix04

mlz=246.5-247.5 F: - cESI SRM [email protected] t246.50-247.50.-272.50-273.50i MSMatrix(X

02113107 09:38;15

RT:8.43AA:10471

o

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f '+ +41,(re)

1001

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RT:6.78AA:33233

RT:4.33AA:49753

RT: 8.32

^d'|22537

RT:5.02AA:13436

AA:80921

PT. t E?

M:,4324

C:\Xca libur\...\MAT_Negative\Matrix05

10q

,tl

02113107 09:49:09

NL:3.45E3n/z=272.5-273.5 F:. cESI SRM ms2

lit?8.@;i.Ht272.50-273.s01 MsMatrix05

NL: 1.66E4rvz= 299.5-300.5 FESI SRM ms2

i33:38ffi3r325.50-326.501 MSMatdx0S

: 4.35E3rVz= 3'l 1.$312.5 F; - cESI SRM [email protected] I311.50-312.50t MsMatnx0S

{o4

@oo

o

_ao

:3.19E3m.tz= 282.E-284.3 F'. . cESI SRM [email protected] I282.7$284.251-MSMatdx05

( 4t*\

C :l(calib ur\...\MAT_Negative\Matrix05

RT:1.15RT:0.85AA:'170i

AA: 174569l

MA:16635

2ooc^ 02113107 09:49:09 'Matrix 10 ("50 ppm.) \),0

NL:3.4583rol

-l

rr'Jz= 272.5-273.5 F: . cESI SRM [email protected]

ms2!_5.99 t246.50-247.50.

272.50-273.501 MsMatnx0S

NL: 1.68E4ffz= 299.5300.5 F: - cESI SRM ms2

ti3 339J3 33 r

325.50-326.50t MsMatrix0S

10(

9l

ar

8C

75

70

9.0

2.71E3rVF 325.5-326.5 F: - cESI SRM [email protected] t sMatrixoS

ooo

Io

-qo

{e +vr,

/s, )

1{L:8.44E2nlz= 282.8-28/.3 F: - cESI SRM ms2

13!:?&_9lf39t",m/z= 3'1 1.$312.5 F: . cESI SRM [email protected] I311.50-312.501 MSMatrix05

C :U(calibur\...\MAT_Negative\Matrix06

NL:5.45E4rvz= 299.5-300.5 F: . cESI SRM [email protected] |299.50-300.50.-325.50-326.50i MsMatrixo6

-NL: 6.39E3

m/z:2465247.5 F: - c

371'*;g1f H.l272.5G273.501 MsMatrix06

1001

,5-l

'oJr5-j

eo-..1

'JI

roJ

oc-lo ^^l"""-]

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331?l_gJfi3lr",

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C :\XcalibuA...\MAT_Negative\Matrix0702113107 10:10:S4

rnlz= 272.5-273.5 F: - cESI SRM ms2ms2

1s.00 [

50 ppm EDTA

RT:0.78AA:r00-l

q<-l*l3?l:3391i33272.50.273.sol272.50.273.501 MsMatdxoT

1 ftjlz=282.8-2A43F:-cESI SRM [email protected] [282.79284.251-MSMatix0T

rvz: 299.$300.5 F: - cESI SRM ms2

It3339J333r325.50-326.501 MSMatrixoT

rvz= 325.5-326.5 F: - cESI SRM msz

t63339J333r325.50-326.50t MSMatnxoT

miz= 3'11.5-3'12.5 F: . cESI SRM [email protected] l311.50.312.501 MSMalrix0T

ooJ

€oao

10G1

^-l'"-l--lru-J

r-ltrlto-]

*lro-l

*ls-l*l45-.{

,^lt:l"l?NJ'-t

taq( a

(*r)

NL:2.69E4rnlz= 246 .*247 .5 F : - cESI SRM ms2291.20@'15.00 |3ZtZ391iH.r272.50-273.sot MsMatrix0T6

I7

70

oo

C :\Xcalib u r\...\MAT_Negative\Matrix0802113107 10:21:43 50 ppm EDTA

0.81o.78RT:

AA: NL:5.8885

29120@'t5246.50-247

ms2r5.00 I

rr/z= 272.1273.5F: - cESI SRM ms2

RT:AA: NL: 2.34E4

r/z= 299.$300.5 F: - cESI SRM ms2

!333&€J333r325.50-326.50i MSMatrix0S

r09

246.50-247.50.'272.50-273.s0t MsMatrix0S

ffilz=246.1247,5F: - cESI SRM ms2

72]6.391 :3.r272.50-273.50t MsMakixoS

6e +*.

RT:8.55AA:23320

RT:5.41M:15034

Io

f

eoao

RT: 1.35

n/z= 311.5-312.5 F; . cESI SRM [email protected] [311.50-312.501 MSMatrixoS

1+at)

C :\j(calibuA...\MAT_Negative\Matrix090?/13107 10:32;34 50 ppm EDTA rxp

- tuRT:M:

0.78 NL:4.27E5rnlz= 272.5273.5 F:. cESI SRM [email protected] r246.s0.247.s0.'zzz.so.zzg.soi rr,rsMatrix09

NL: 7.48E3m/z= 299.5-300.5 F: - cESI SRM ms23/t4.20@15,00 t299.50-300.50,-325.50-326.501 MSMatrix09

RT:AA:

0.811001

ss-l

100

90

: 5.48E3rYz= 325.5-326.5 F:. cESI SRM [email protected] [299.50-300.50.-325.50-326.501 MSMatrixo96

80

a

RT:2.12Ai\:17290

oI6

a

.E

RT:0.89M:7072

RT:8.20AA:23505

filz= 282.6-2U.3 F:. cESI SRM [email protected] I282.75-2U.251 MS

ms21s.00 I

NL: '1.68E3

rvz= 31 1.5-3'12.5 F: - cESI SRM [email protected] [311.50-312.50t MSMatrix09

C :\lXcalibur\...\MAT_Negative\Matrix 1 0 02113107 10:43:28 50 ppm EDTA

RT:M: NL:2.64E5

nlz=272,5-273.5F: - cESI SRM [email protected] I246.50-247.50.'272.50-273.50i MSMatrix'|0

otr6

!

o.:Go

NL:4.87E3r/z= 31 1.5-312.5 F:. cESI SRM [email protected] l311.5G312.50t'MSMatrix'10

{^t Hu(+t)

1001

nl'l'lro1

7l7o-]

os]

1ocr

'"J"-J'lro-l

'-lzo-]

*-luo-1

*l*-l,u-l

40J

^-lJl.o-]

rilz= 325.5-325.5 F: - cESI SRM [email protected] t299.50.300.50.-ses.so-sze.soi l"tsMatrixl0


rol95-.{

*.]85-l

rol

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o ^^l9",-]

1 00-^-l*le0-1

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fiYz= 325.$.326.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSMatrixl l

ESI SRM [email protected] [311,50-312.501 MSMatrixl l

{*qt

C :XcalibuA...\MAT_Negative\Matrix 1 2

1001

*l

0Z13lO7 11:05:13

'n,lz=272.*273.5F: -cESI SRM [email protected]

ms2r5.00 [

246.50-247.fi,272.50-273.50t MSMatrixl2

Matrix 2 ("500 ppm') nx(,0.1

RT:MA:

NL: 8.32E4r/z= 299.5-300.5 F: . cESI SRM [email protected] I299.50-300.50.325.50-326.501 MSMatrixl2

nl/z= 246.$.247.5 F: - cESI SRM [email protected] I246.50.247.50.272.50.273.501 MSMatdxl2

o3

€o

6

4.1 7E3nvz: 311 .t312.5 F: . cESI SRM [email protected] [3't '1.50-312.501 MSMatrix 12

fouqa

C:U(calibur\...\MAT_Negative\Matrixl 3 0?/13107 11:16:02 Matrix 3 ("500 ppm") qlp

rol

'l*-J'l1.1'l701

.'-]I ^*l

tnlz=246.5-247.5 F: - cESI SRM [email protected] [246.50-247.fi.272.s0-223.50i MsMatnxl3

fl,t'tt,

rvz= 31 1.5-312.5 F: - cESI SRM [email protected] I311.50-312.501 MSMatrixl3

rf'lz= 262.&1943 F: - cESI SRM [email protected] I282.7*28{251 MSMatrix'13

(4 3)

C :U(calibu r\...\MAT_Negative\Matrix 1 4 02J13107 11'.26:52 Matrix 4 ("500 ppm')

RT:4.25M:24620

RT:3.18AA:1E839

RT:1.15MA:2097890

RT: 1.27AA:1194082

NL:3.67E4rnlz= 299.$300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.50t MSMatrix'14

100r

,'-1

rnlz= 272.12735F: - cESI SRM [email protected] [246.50.247.50.272.5S273.501 MSMatrix'14

nlz= 242.8-2U3 F: - cESI SRM [email protected] I282.7r2U.251 MSMatrixl4

RT:6.78AA:27941

RT:7.7816

I

€o

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NL: 5.02E3rvz= 31 1 .t312,5 F: - cESI SRM [email protected] I311.50-312.50t MSMatrixl4

: 1.49E4

RT: '1.'15

fuqte,

RT: 4.12M:10676

C :\jXcalibur\...\MAT_Ne gative\Matrix 1 S 02/13n7 f:37:47<Jhg

NL: 4.94E4rnlz= 299.5-300.5 F: - cESI SRM [email protected] |299.50-300.50.-325.50-326.501 MSirlatnx'15

RT:6.86AA:54615

pT. ? na3562 RT: 5.10

AA: 50970

10(

80

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65

RT:0.93AA:138673

RT:3.84AA: 38576

RT:7.36AA:24214

Io

leo5oo

RT:6.06AA: 18141

RT:6.28AA:7102

5. q,/U

/ 4'.)

RT:2.57

Nz= 282.8-2U.3F: - cESI SRM [email protected]$2U.251 MSMatnxlS

: 1.78E3

C :Xcalibur\...\MAT_Negative\Matrix,t 6 02113107 11:48:42

RT:0.8S.rol*"rt*

'llNL:2.1286rnle 272.5-273.5 F: - cESI SRM ms2

lit?P;i#l272.50-273.501 MSMalix'16

oo

o

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ntz= 282.8-28(.3Fl. - cESI SRM [email protected] t282.7$284.251- MSMatrixl6

5.qru(+t)

clop- tuRT:AA:

0.89NL: 2.31 E5rvz= 299.$.300.5 F: - cESI SRM [email protected].'325.50.326.501 MSMatrixlS

: 4.38E3r/z= 325.5-326.5 F: - cESI SRM [email protected].'325.50-326.50t MsMatnxl6

RT: 1.27M:11820

RT:4,18AA:4894

C:U(calibur\...\MAT_Negative\Matrix I 7

RT:0.85AA:

100

90

NL:2.29E6trtz= 272.5-273.5 F: - cESI SRM [email protected] I246.s0. ,47.50.'272.50-273.50t MSMatrixlT

.'].lz= 246.5-247.5 F: - cESI SRM ms2

3il33g.'i33r272.50-273.501 MSMatrixlT

NL:2.5685trVz= 299.5-300.5 F:. cESI SRM [email protected] I299.50-300.50.'325.50-326,501 MsMatrix'17

m/z= 325.5-326.5 F: - cESI SRM ms2

i33339J333r325.50-326.501 MsMatnx'|7

0213107 11:59:36 500 ppm EDTA

RT:AA:

AA:29498

8

80RT: 0.86AA:38925

70

oc

oP

€@

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RT:1.73AA:

M:4728trVz= 31 1.5-312.5 F: . cESI SRM [email protected] I311.50-312.501 MsMalixlT

O,t4,/6io ( qtt\

C :\Xcatib u r\...\MAT_Neoative)gllx,lg_

't001

*t

AA:926981

fiilT= 272.*273.5 Ft . cESI SRM [email protected] [246.50-247.50.272.5G273.501 MSMatrixlE

.':r'z= 246.1247.5 F: - cESI SRM [email protected] [246.50-247.50.zzz.so-zzs.sol usMatflx18

mlz= 282.6284.3 F: - cESI SRM [email protected] [282.7U2U.251 MSMatrixlE

0?J13107 12:10:25 500 ppm EDTA

0.89

. tuRT:M: RT:

AA:

0.851511 NL:2.3385

rvz= 299.$300.5 F: - cESI SRM [email protected].'325.50-326.501 MSMatrixlS

oI6

J

{oEso

100

VJ

80

T'

70

ft+,+a

C:U(calibur\...\MAT_Negative\Matrix 1 9

1 00-

ar-l

RT:AA:

neE15f E

NL: 1.42E6ffilz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50,?72.s0-273.50t MSMalrixl9

NL: 2.82E5m2= 299.5-300.5 F: - cESI SRM [email protected] I299.50.300.50.325.50-326.50i MSMatrixl9

02113107 12:21:15 500 ppm EDTA <l-D6

RT:3.72AA:19293

o

€o

-qo

GDfFlroi-l

RT:4.56AA:6280

NL:3.99E3rr'lz= 282.A-2U3F: - cESI SRM [email protected] [282.7r2v.25t MSMatrixl9

44a

r/z= 311.5-312.5 F: - cESI SRM [email protected]'1.50-312.s01 MSMatnxl I

NL:6.55E4atz= 245.$247.5 F: - cESI SRM [email protected] I

(vtr)

C:l(calibur\...\MAT_Negative\Matrix2002113107 12:32:06

NL:1.67E6ntlr272.5-273.5F: - cESI SRM [email protected].'272.50-273.501 MSMatnx20

0.85169r

RT:AA: RT:0.96

,Qq:NL:2.18E5rnlz= 299.5-300.5 F: . cESI SRM ms2ms2

r5.00 I133339J33,1r325.50-326.50j MS

10(

ol

80

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70

t*r*lM'J*l8s-J

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801

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70-.i

^-l^^lou-'l

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^-l""1'oj

o6

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trYz= 31 '1.5-312.5 F: - cESI SRM [email protected] [311.50.312.501 MSMatrir0

RT:5.38M:6106

Z^L (L4b( vuu)

7.12E3

RT: 3.11AA:'13513

RT: 8.85

Positive lonization Mode- Matrix Effect

EDTA free brood swabs- extracted then spiked to be 50 ppm EDTASampte Area of RIC ior base p""r tifo'*Ll12 33iff3:3 4ffi61154 28409525 12647507

AVERAGE . 6598351.4

Neat EDTA sotution- S0 ppmInjection Area of RIC for base peak (160 m/z)1 5578912 5505153 6155724 9453795 70773gAVERAGE

67s41g

Matrix Effect (50 ppm), % 976.9285687

Injection Area of RtC for base peak (160 m/z)1 59578792 69577583 69839274 62794875 36871037772030.8

EDTA free blood swabs- extracted then spiked to be s00 ppm EDTASample Area of RtC ior base peak (iOOrnlrl1 94101312 2$082973 180804884 229021365 1ilfl570AVERAGE

$169724.4

Neat EDTA sotution- 500 ppm

AVERAGE

Matrix Effect (500 ppm), % 233.7062843

{* +qa r,( u l.,ravF&,a,\

NEGATIVE lonization Mode- Matrix Effect

EDTA free blood swabs- extracted then spiked to be s0 ppm EDTASample Sum of Areas of free EDTA peaks (mtz 273 + 247)1 1706182 744963 791434 $7215 17019AVERAGE B7g4s

Neat EDTA sotution- S0 ppmInjection Sum of Areas of free

1

2

345

AVERAGE

Matrix Effect (50 ppm), %

EDTA free blood swabs- extracted then spiked to be s00 ppm EDTASample Sum of Areas of free EOTA peaks (mlz 273 + 247)1 109622622 p6083183 5697374 21477275 2144609AVERAGE

5766530.6

Neat EDTA solution- 500 ppmInjection

I

2

345

AVERAGE

Matrix Effect (500 ppm), %

EDTA peaks (mtz273 + 247)120675717906604605670395676529014832892267

3.040694376

Sum of Areas of free EDTA peaks (mlz2|3 + 247)147852671 889339216049375168318071 7809391

16873846.4

34.1743694

f* qqn( vva)

zlllt't1-pp

SPOT STZE L.O.D.

6 uuo(v+a)

lw02tr5t2007

Blood spot sizes (l uL, 5 uL, 10 uL)

f* +vb&+v)

Sequence--Spot Size_pos.sfd [OpenJ

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name sample lD Path %Unknown :Spom-

I

1

C : U(ca li b u r\m -I odslEDil-F o s


*****t*******t*t**********t**********

Sample Name:

Comment:

t*******************t****t**l*************t*****************************t**********rr

Study:

Client:

Laboratory:

Company:

Phone:

1uL +A

lnst Method Proc Method CalFile Position InjVol'\Xnelihr r TA_Pos_Swa 2 5.0 j0.000

I


****l********************t**t**************t************************************t**********************************itr

& uo,z/rr/"r

Tl?P(vv;)

Sample Name:

C 'nent:

Seq uence--Spot Size_pos. sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:

:Xcalibur\D@


*********************************t************************************i*******t*************************i*********r********r******i*****f*****

Sample Name:1t-lComment:

-

Study:

Ctient:

Laboratory:

Company:

phone:


**t***************************************************s****************t*******************************i*****i*tr**********************tr*****

f, urc( v+)

>ltr ["rttr{]

Sample Name:

C- -menf

Sequence--Spot Size_pos. sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:

lnst Method Proc Method CalFile Position InjVol

53-Level Sample WttEUtuus\EU lA_f,os_Swabs 1 0.000

***********************************************************t***t***************************t*****************t***************f***************

Sample Name:

Comment:Study:

Client:

Laboratory:

Company:

Phone:

Sample TypG File Name Sample lD Path:Unknown Spot06 04 u. u\cat I our\uata\ts D I A\Brewer\s pot s ize_positive

lnst Method Proc Method CalFile Position lnjVol Level Sample Wt\Xcalihr rr\rnath;;.\trnr^4 5.0 0.000

sample Vol ISTD Amt Dil Factor0.000 0.000 1.000

*******t***********i******ft****H*t*****************************************************t*****************tr***********r*********i************

foq&kvt)

lgl"ts,)p

Sample Name:

C--.rnent:

Seq uence--Spot Size_pos. sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:

A\Brewer\Spot Size_posi


Comment:Study:

Client:

Laboratory:

Company:

Phone:

uL +A

Inst Method Proc Method CalFile Position hJVol Level ple'J(caiiburimeiffic 5.0

Sample Vol ISTD Amt ]Dit Factor

u.000 0.000 1.000

t********t********t*****t***************t**t******************************r*********e*s*

o4-(v

4k-,q4

zlr l'tT]1P

Sample Name:

C^-.ment:

Sequence--Spot Size_pos.sld [Open]

blood swab extract

Study:

Client:

Laboratory:

Company:

Phone:

C:U(calibur\De


0.000 0.000 1.000

*******************i********************t*******i***t*************************************s******t*************************it************t*

Sample Name:

Comment:

5ULEDTA+B

Study:

Client:

Laboratory:

Company:

Phone:


0.000 0.000 1.000

f" uu"(u+r)

zls l,t5vp

Sample Name:

? rtent:

Sequence---Spot Size_pos. sld [Open]

Neg blood swab extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown Spot11 01 C :U(cal ibu r\OataE Otn@

lnst Method Proc Method Cal File Position InjVol Level Sample WtC :U(cali bur\metho0G\EDTn pos5vabs

1 5.0 0.000


0.000 0.000 1.000

Sample Name:

Comment:

5 uL EDTA +

Study:

Client:

Laboratory:

Company:

Phone:


Unknown Spot12 07 C: \)(cal i bur\Data\E DTA\eretedS pof S ite positive

Inst Method Proc Method Cal File Position InjVol Level Wt7 5.0 0.000


0.000 10.000

1.000

CC'/ 4fu(+s")

zlrrl"'tg)p

Sequence--Spot Size_pos.sld [Open]


Study:

Client:

Laboratory:

Company:

*******t****************f ****t*********i************ ****t*************l

TPFSample N

Comment:

10 uL EDTA + A

Study:

Client:

Laboratory:

Company:

Phone:

lSample Wt

8" +tt'zlrr("1

5W)

( vs)

Sequence---Spot Size_pos.sld [Open]

Sample Name:

C- 'nent:

blood swab extract

Study:

Client:

Laboratory:

Company:

Phone:

Sample Name:

Comment:

1O uL EDTA +T0flStudy:

Client:

Laboratory:

Company:

Phone:

***************t****t** *******t********************************t*i*********

LL q4b(v:4

>hr l"t./tp

Sequence--Spot Size-pos.sld [Open]


*****l**l*************t*****************

Sample Name: 1O uL EDTA + C

Study:

Client:

Laboratory:

Company:

Phone:

**i*i***a*****************t*************i************t***********f*s*****i*****

$FComment:

*******tt**************************************t*******

Study:

Client:

Laboratory:

Company:

Phone:

t* ++ai\t' 4S) \'/

nana O

> ls 1"1

1p

I Sample Wt

Sample Name:

C-'-nent:

Sequence--Spot Size-pos. sld [Open]

swab extract

Study:

Client:

Laboratory:

Company:

Phone:

**t*********a******i****t***i*it**********t*********************t****************************

*. 51''? f@

54-rots €2;24€^/ cG' &€TL 9," L wil ,

u"rttt€ fttCd^4zer-/ ot1eczeV .

(/Nctr { ^C

lhr

t* qon( v'4

vlrrl't5'rP

C:l(calibur\...\Soot0 1 0A15107 1'l:46:31

nvz= 159.$160.5F: + c ESI Full [email protected] [125.00-315.001 MSSpotol

293.00@1 5.00 [ 1 25.00€1 5.00]151

ms2Full

nlz-246.sl47.5F: + c ESI Full [email protected] I125.00-315.001 MSSpotol

t+-+a('/t)


0?i15107 11i57'.42

NL:2.79E4nvz= '159.5-'160.5F: + c ESI Full [email protected] I125.00-315.001 MSSpot02

f* qqo

ftl


C:U(calibur\...\SpotO3 02115107 12:08:34

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Seq uence---CT_Spot_neg. sld [O pen]

ive Blood extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown cTo1 1 U(calibu AData\EDTA\Brewer\CT_N egative

Inst Method Proc Method CalFile Position lnjVol Level Sample Wtu : \xca | | bur\methods\EDTA_Neg_swabs 11 5.0 0.000


0.000 0.000 1.000

Sample Name: t-_Comment Study:

Client:

Laboratory:

Company:

Phone:

sample Iype File Name Samole lD Path

Unknown cT02 01 C: U(cal ibu AData\EDTA\BreweACT_N egative

nst Method Proc Method Cal File Position InjVol mple WtC : U(cal i b u r\methods\EDTA_N eg_Swabs I 5.0 0.000


0.000 0.000 1.000

*********************t************

/QY

,\tt t'"fo uno(+'t)

Sample Name:

" .nent:

Sequence---CT_Spot_neg. sld [Open]

Negative Blood extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown cTo3 11 C:Xcalibu AData\EDTA\Brewer\CT_Negative

Inst Method Proc Method CalFile Position lnjVol Level Samole WtC :\)(calibu r\method s\E DTA_N eg_Swabs 11 5.0 u.u00


0.000 0.000 1.000

*i*i*t****t*********t****ff **********

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT04 11 C :Xcali bu r\Data\E DTA\Brewer\CT_Negative

Inst Method Proc Method Cal File jPosition InjVol Level lSample Wt

C:Xcalibur\methods\EDTA Neo Swabs 11 5.010.000


0.000 U.UUU I.UUU

-tbs

r,\rj\"t+qb

I!:?

Sample Name:

c rent:

Seq uence---CT_Spot_neg. sld [Open]

JC2neg

Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT05 02 C : Xcali bu r\Data\EDTA\Brewer\CT_Negative


C :U(ca libu r\method s\E DTA_N eg_Swabs 2 5.u 0.000


0.00u O.UUO 1.000

t*t*********t*****************t**********************************t*****r********i**t**

Sample Name:

Comment:

extract

Study:

Client:

Laboratory:

Company:

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UNKNOWN cT06 11 lC:U(calibur\Data\EDTA\Brewer\CT_Negative

lnst Method Proc Method Cal File Position InjVol Level tSamole Wt

C :Xcal ibu r\methods\EDTA_N eg_Swabs 11 i5.0 0.000

sampre vol ISTD Amt Dil Factor

0.000 0.000 1.000

{* uq,(+")

nana ?

-1vP

1\..(\'1

Sample Name:

C rent:


Blood extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown cTo7 11 C:U(calibuAData\EDTA\Brewer\CT tteoative

Inst Method Proc Method CalFile Position llnjVol Level Samole Wt:Xcal i bu r\methods\E DTA_Neg_Swabs 4atl 5.0 0.000


0.000 0.000 1.000

Sample Name: JC3neg

Comment: Study:

Client:

Laboratory:

Company:

Phone:


Unknown iCT08 03 C : \Xcalibu r\Data\E DTA\Brewer\CT_N egative

nst Method Proc Method Cal File Position llnjVol Level ;Sample Wtv. \/\sailour\melnoos\tr u I A_Neg_ ? 5.0 0.000

mple Vol ISTD Amt Dil Factor

0.000 0.000 1.U00

€o q,/ b(,/%)

n^da l

Rq

1lt(\"1

Sample Name:

C rent:


extract

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Narne Samole lD Path

Unknown cT13 11 C : U(cal ibu AData\E DTA\Brewer\CT_Negative

Inst Method Proc Method CalFile Position lnjVol Level Samole WtC:U(ca libu r\methods\EDTA_Neg_Swabx 11 5.0 0.000


0.000 0.000 1.000

Sample Name:

Comment:

JC5neg

Study:

Client:

Laboratory:

Company:

Phone:


unKnown cT14 05 :Xcalibur\Data\EDTA\Brewer\CT Neoative

Inst Method Proc Method CalFile Position InjVol Level Sample WtC : \Xca li b u r\methods\E DTA_Neg_Swa bs 5 5.0 0.000


0.000 0.000 1.000

l***********************t***t**************t*t*******t***********

f, +q,(+ tr)

nana 7

-1rq

,\,,\"

Seq uence--CT_Spot_neg. sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:


Unknown T11 04 C:U(calibur\Data\EDTA\Brewer\CT Neqative

Inst Method Proc Metnod CalFile Position InjVol Level Samole Wt

C :U(calibu r\methods\E DTA_Neg_Swabs 4 5.0 0.000


0.000 0.000 1.000

********************t****t******t******a*******t

Sample Name:

Comment:


Study:

Glient:

Laboratory:

Company:

Phone:

a**r*******t****r**


Unknown cT12 11 C :U(calibu r\Data\EDTA\Brewer\CT Neqative

lnst Method Proc Method Cal File Position InjVol Level lSample Wt

C : U(calibu Amethod s\EDTA_N eg_Swabs 11 r5.0 0.000


0.000 0.000 I.UUU

,$e

, \,.(\orf* +,/ (-(,t1;D

Sample Name:

c 'nent:


extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT09 11 C :U(calibu r\Data\E DTA\BreweACT_Negative

Inst Method Proc Method Cal File Position InjVol Level Samole Wt

C : U(ca li bu r\methods\E DTA_N eg_Swabs 11 5.0 0.000


0.000 0.000 t.utlu

**********i**********t************************tr******************t********t*t*****************t**t*t*****t**********************************

Sample Name:

Comment:

extract

Study:

Client:

Laboratory:

Company;

Phone:


Unknown cT10 11 C : Xcalibur\Data\E DTA\Brewer\CT_N egative


C : U(cal i bu r\methods\E DTA_Neg_Swabs 11 5.010.000


U.UUO 0.000 1.000

**a****i***t****t******t**t***********t******************tt**s*************

fuqau

^^(

u.' u)

,/r ut

-t\"\"'

Sample Name: Negative Blood extract

r rent:


Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT15 11 : Xca I ibu r\Data\EDTA\Brewer\CT_Negative

Inst Method Proc Method CalFile Position lnjVol Level lSample WtC :U(cal i bur\method s\EDTA_Neg_Swabs 11 5.U u.000


0.000 0.000 1.000

*********************

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT16 11 C:Xcalibur\Data\EDTA\Brewer\GT Neoative

Inst Method Proc Method CalFile Position InjVol Level Samole WtC : U(cal ibur\methods\EDTA_Neg_Swabs 11 5.0 r0.000


0.000 0.000 1.000

CCv 44Cz\( 47+S

.'ivq

)t.""''

Sample Name:

c nent: Study:

Client:

Laboratory:

Company:

Phone:

Seq uence---CT_S pot_neg. sld [Open]

Sample rle Name Sample lD Path

Unknown CT17 06 C :XcalibuAData\E DTA\Brewer\CT_Negative

Inst Method Proc Method CalFile Position InjVol Level Sample WtC :\)(cali bu r\methods\E DTA_Neg_Swabs 6 5.0 0.000


0.000 0.000 1.000

****t***********r*t*********t****r

Sample Name:

Comment:


Study:

Client:

Laboratory:

Company:

Phone:

*******************


Unknown cT18 11 C : Xcalibu AData\EDTA\Brewer\CT_Negative


C :Xcalibur\methods\EDTA_Neg_Swabs 11 5.0 0.000


0.000 0.000 1,000

CLu 44b(vts)

naaa O

11..'"

Sample Name:l Negative Blood extract

t' rent:


Study:

Client:

Laboratory:

Company:

Phone:


unKnown cT19 11 C:XcalibuAData\EDTA\Brewer\CT Neoative

Inst Method Proc Method CalFile Position lnjVol Level lSample Wt

C :U(calibur\methods\E DTA_N eg_Swabs 11 5.0 0.000


0.000 0.000 1.000

****t****t**+**************t****t*****1

Sample ttame:

Study:

Client:

Laboratory:

Company:

Phone:


Unknown f20 07 C : Xcalibu AData\EDTA\BreweACT_Negative

lnst Method Proc Method CalFile Position InjVol Level Wt

C:Xcalibur\methods\EDTA Neo Swabs 7 5.0 i0.000


0.000 0.000 1.000

*******************t

11 ,''-'[o qq,(vto)

nana 1O

Sample Name:

C rent:


extract

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name Samole lD lPath'l

Unknown cT21 11 :U(calibur\Data\EDTA\Brewer\CT Neoative




0.000 0.000 1.000

*****tt****t**

Sample Name:

Comment:

extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown CT22 11 C:U(calibur\Data\EDTA\Brewer\CT Neoative

lnst Method Proc Method Cal File Position InjVol lLevel lSample Wt



0.000 u.uuu I 1.uuu

,sq

[) q,t,- r\'(\"1(vzt)

naaa 14

Seq uen ce--CT_Spot_neg. sld [O pen]

Study:

Client:

Laboratory:

Company:

Phone:


Path

Unknown cr23 108

C :U(calibu AData\EDTA\Brewer\CT_N egative

lnst Method Proc Method CalFile Position nJvol Level Samole Wt

C :U(ca I i bu r\methods\E DTA_N eg_Swabs 8 5.0 0.000


0.000 0.000 1.000

Sample Name:

Comment:

ative Blood extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT24 11 C :U(calibu r\Data\EDTA\BreweACT_N egative

nst Method Proc Method CalFile Position lnjVol Level lSample Wt

C :U(cal ibur\methods\EDTA_Neg_Swabs 11 5.0 0.000

{otL\,i\'1f* q'/o

--(:"'^t)

Sample Name:

r lent:



Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT25 11 C :Xca I ibu r\Data\EDTA\Brewer\CT_Negative

lnst Method Proc Method CalFile Position InjVol Level Sample Wt11 b.u 0.000

Sarnple Vol ISTD Amt Dil Factor

u.000 0.000 1.000

Sample Name:

Comment:

JC9neg

Study:

Client:

Laboratory:

Company:

Phone:


Path

Unknown cT26 09 C : U(cal ibu r\Data\EDTA\BreweACT_N egative

Inst Method Proc Method CalFile Position InjVol Level lSample WtC :Xcal i bu r\methods\EDTA_Neg_Sw{ 5.0 0.000


0.000 0.000 1.000

'sns

v\t(\"14 *.,lvtq\'/

Sample Name:

r *nent:

Seq uence---CT_Spot_neg. sld [O pen]


Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT27 11 C:Xcalibur\Data\EDTA\Brewer\CT Neoative

Inst Method Proc Method CalFile Position njVol Level Sample WtC :U(calibur\methods\EDTA_Neg_Swa bs 5.0 0.000


u.0u0 0.000 1.000

*********t*********t*t************f**********************t****t*****t****t****i************t***t********t**********************i*********t*t*t

Sample tlame:

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type File Name samDle lu Path

Unknown cT28 11 C:U(calibur\Data\EDTA\Brewer\CT Neqative


:Xcalibur\methods\EDTA Neo Swabs 11i5.0 r0.000


0.000 0.000 1.000

*i**************

[v aqb(:,n.)

-frrq

)\'.i \:r


Sample Name:

r rent:

0neg

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type ile Narne lSample lD Path

Unknown cT29 10 C : U(cal ibur\Data\EDTA\BreweACT_Negative

Inst Method Proc Method CalFile Position InjVol Level Sample WtC :Xcal ibu r\methods\E DTA_N eg_Swabs 10 5.0 0.000


0.u00 0.000 1.000

Sample Name:

Comment:

ive Blood extract

Study:

Client:

Laboratory:

Company:

Phone:

$ample lype File Name Sample lD Path

Unknown cT30 11 C : U(calibur\Data\E DTA\BreweACT_N eg ative

ample Vol STD Amt lDil FactorI

0.000 0.000 1.000

fo u+a(+t,)

{1t,t.<\r

Sample Name:

C rent:


extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown cT31 11 ; : \Xcalibu r\Data\EDTA\Brewer\CT_Negative

Inst Method Proc Method CalFile Position

iT-InjVol Level Sample Wt

C:\)(calibur\methods\ED1a_Neg:Swebi 5.O U.UOO


0.000 0.000 1.000

t******t***********t******t*******t************************t*t*************t***********st***********r**ti**********************r************

Sample Name:

Comment:

Pos. Control EDTA btood eitStudy:

Client:

Laboratory:

Company:

Phone:


Unknown CT32 12 C : U(cali bu r\Data\EDTA\BrewerEfl*.|egaiite

Inst Method Proc Method CalFile Position lnjVol Level Sample Wtu : \xcat I bu r\methods\E DTA_Neg_Swabs 12 5.0 10.


0.000 0.000 1.000

**********i**************************************t****i***t***************************i***

€u'/va

!u:')

,-\!t

)\r(\-n

Sample Name:

. nent:



Study:

Client:

Laboratory:

Company:

Phone:

Sample Type ile Name Sample lD Path

Unknown 11 G :U(calibuAData\EDTA\Brewer\Spot Size_Negative

nst Method Proc Method Cal File Position njVol Level Sample WtG:Xcalibur\methods\EDTA Neo Swabs 11 5.0 0.000


U.UOU 0.000 1.000

Sample Name:

Comment:

1uL EDTA+ A

Study:

Client:

Laboratory:

Company:

Phone:


Unknown lSpotOl 13 C :U(calibu AData\EDTA\B rewer\Spot Size_Negative

Inst Method Proc Method CalFile Position njVol Level lSample WtI

C : Xcal i bu r\methods\EDTA_Neg_Swabs 13 5.0 0.000


0.000 0.000 1.000

LX(4

UWa(")

'int ^" '\a I

.. \.s'

Sample Name:

r nent:

Sequen ce---CT_Spot_neg. sld [Open]

ive Blood extract

Study:

Client:

Laboratory:

Company:

Phone:


Unknown SpotO1 11 C:U(cal ibu r\Data\EDTA\Brewer\Spot Size-Negative

Inst Method Proc Method CalFile Position InjVol Level Sample WtC : U(calibur\m eth od s\EDTA_Neg_Swabs 11 5.0 u.000


0.000 0.000 1.000

***************

Sample Name:

Comment:

1uL EDTA+ B

Study:

Client:

Laboratory:

Company:

Phone:


Unknown SpotO1 14 C : U(cali bu r\Data\EDTA\BreweASpot Size_Negative

t******r**t*********

44t 2-{$$

-t,ut"'( 4s1)

Sample Name: Negative Blood extract

f lent:

Seq uence---CT_Spot_neg, sld [Open]

Study:

Client:

Laboratory:

Company:

Phone:

Samp Frle Name Sample lD Path

Unknown Spot01 11 C:U(cali bu r\Data\E DTA\Brewer\Spot Size_N egative

lnst Method Proc Method ual Frle Position InjVol Level Samole WtC:Xcalibur\methods\EDTA Neq Swabs 11 5.0 U.OOU


0.000 U.UUU r.000

***************************t**t*****************t********t*t***

Sample Name:r-"'-lComment: Study:

Client:

Laboratory:

Company:

Phone:

Sample Type Ftle Name Samole lD Path

Unknown SpotO1 15 C :Xcali bu r\Data\EDTA\Brewer\Spot Size_N egative

Inst Method Proc Method CalFile Position lnjVol Level lSample WtC:U(calibur\methods\EDTA Neo Swabs 15 5.0 0.


0.000 0.000 1.000

& q,to( +rs)

n^Cl'v\' -\o I

r,\\J

Sample Name:

(' nent:



Study:

Client:

Laboratory:

Company:

Phone:


Unknown Spot01 11 C : Xcal ibu AData\EDTA\B rewer\Spot S ize_N egative

lnst Method Proc Method CalFile Position InjVol Level jSample WtI

C:U(calibur\methods\EDTA Neo Swabs 11 5.0 u.u00


0.000 0.000 1.000

.tSample Name:

Comment: Study:

Client:

Laboratory:

Company:

Phone:


Unknown SpotO1 to C :\)(cali bu r\Data\EDTA\B rewer\S pot S ize_N egative


C:Xcalibur\methods\EDTA Neo Swabs 16 b.u 0.000


U.UUU rJ.u00 1.000

**************t*************tt****t*t***************** a**************t*****

q+C2

1r^:r>'\nR,ra

r\$'

Sample Name:

r nent:


Study:

Client:

Laboratory:

Company:

Phone:

extract

Sample Type l-rle Name Sample lD Path

Unknown Spot01 11 C:Xcali bu AData\EDTA\Brewer\Spot Size_Negative

Inst Method Proc Method Cal File Position lnjVol Level Sample Wt

: U(calibu r\methods\E DTA_Neg_Swabs 11 b.rJ U.OOU


0.000 0.000 t1.000

Sample Name:

Commenl

SuL EDTA+ B

Study:

Client:

Laboratory:

Company:

Phone:


Unknown iSpotOl 17 C :Xcalibu AData\EDTA\Brewer\Spot S ize_Negative

lnst Method Proc Method Cal File Position InjVol Level :Sample Wt

C:Xcalibur\methods\EDTA Neq Swabs 17 b.0 0.000


0.000 0.000 1.000

&qqn11,1'"( vsz)

Sample.Name:

t' nent:



Study:

Client:

Laboratory:

Company:

Phone:


Unknown SpotO1 11 :Xcal i bu r\Data\EDTA\BreweAS pot Size_N egative

Inst Method Proc Method CalFile Position InjVol Level Sample WtC:U(calibu r\methods\E DTA_N eg_Swabs 11 5.0 0.000


0.000 0.000 1.000

Sample Name:

Comment:

5uL EDTA+ C

Study:

Client:

Laboratory:

Company:

Phone:


Unknown SpotO1 18 C:Xcalibu AData\E DTA\Brewer\S pot Size_N egative

Inst Method Proc Method CalFile Position InjVol Level lSample Wt

C :Xca I ibu r\method s\E DTA_N eg_Swabs 18 5.0 0.000


0.000 0.000 1.000

(/ rl (-(+s)

aaaa )r)

1\,rJrr\'. '

Sample Name:

C -rent:



Study:

Client:

Laboratory:

Company:

Phone:


Unknown Spot01 11 C : U(calibu r\Data\EDTA\Brewer\S pot Size_t tegative

Inst Method Proc Method CalFile Position InjVol Level Sample Wt; : \Xca I I bu r\methods\E DTA_N eg_Swabs 11 5.0 0.000


0.000 0.000 1.000

****t*******************t****t**************************t*****t************t**r*********************************************r*****i*t*****i

Sample Name:

Comment:

1OuL EDT

Study:

Client:

Laboratory:

Company:

Phone:


Unknown Spot01 19 :Xcal i bu r\Data\E DTA\Brewer\Spot S ize_frlegative

Inst Method Proc Method Cal File Position InjVol Level Sample WtC :U(ca I i bu r\m ethod s\EDTA_Neg_Swa bs 19 5.0 0.000


U.UUO 0.000 1.U00

r*************i************

C4L qqG/\(Vs'iS

st,,,..,4/\r'

Seq uen ce---CT_Spot_neg. sld [Open]

Sample Name:

c rent:


Study:

Client

Laboratory:

Company:

Phone:


Unknown SpotO1 11 C :U(cali bu r\Data\E DTA\Brewer\Soot S ize N eo ative

Inst Method Proc Method CalFile Position InjVol Level Samole Wt


sample vol ISTD Amt DilFactor

0.000 0.000 1.000

***+********************t*************t*********************

Sample Name:

Comment: Study:

Client:

Laboratory:

Company:

Phone:

1 *


Unknown Spot01 20 C : U(cali bu r\Data\EDTA\Brewer\Spot Size_N egative


C : U(calibu r\methods\EDTA_Neg_Swabs 20 5.0 0.000


O.UUU 0.000 1.000

********************t****r

6r++t-('/ q,) {\\*.1

V\

Sample Name:

C nent:



Study:

Client:

Laboratory:

Company:

Phone:

C:Xcalibur\Data\EDTA

Sample Vol ISTD Amt Dil Factor0.000 0.000 1.000

*************************************************************************i*********t**t************r***i******t****.****************************t

Sample Name:

Comment:

1OuL EDTA+

Study:

Client:

Laboratory:

Company:

Phone:

nst Method Proc Method ual Ftle Position InjVol Level Sample WtA_Neg_ 12 5.0 0.000


0.000 0.000 1.U00

*****t********************t*******t****************i*******t***********t***$******i***i*******i**********t****t*******

5r,/,/a(\:,) .i$$,1o1

-\i

Sample Name:

C '"nent:


extract

Study:

Client:

Laboratory:

Company:

Phone:

Sample Type rle Name Sample lD Path

Unknown Spot01 11 C :U(cal ibu r\Data\E DTA\BreweASpot Size_Negative

Inst Method Proc Method CalFile Position InjVol Level Sample WtC :U(ca libu r\methods\E DTA_Neg_Swabs 11 5.0 0.000


u.00u 0.000 1.000

**************** *************ft**#*

fi v+o(48, 1l'+^

C:\XcalibuA...\Spot Size_Negative\Ct33 02116107 03:47:38

rlz= 272.5-273.5 F: - cESI SRM [email protected] [246.sO-247.50,272.50-273.501 MSc133

121E3mlz= 246-t247.5 F: - cESI SRM ms2291 [email protected]

ms2t5.00 [

246.50-247.50.272.50-273.s01 MSct33

Negative Blood extract TtBNL: 1.42E3nvz: 299.5-300.5 F: - cFSI SRM [email protected] I299,50.300.50,325.50.326.501 MScr33

Q

d

€og@

.I]/z= 282.a-28r'.,3 F'. - cESI SRM [email protected] [282.7r2U.251 MSct33

5r 4+o

C:\i(catibuA...\Spot01 oz16t\7 03:58:32 1 uL EDTA+ A

-llesJ Itlt

'-1 ll

: 4.43E3nlz=246.1247.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSpotol

nlz= 282.8-2U.3 F: - c

: E.55E3ff|/z= 325.5-326.5 F: - cESI SRM [email protected] MSSpoto l

o

6c

qo

ESI SRM [email protected] [282.7$284.251 MSSpoio'l

Time (min)Time (min)

froo,

C:XcalibuA. .\Spot01_0702 1 6040921|..-- 02116107 04:09:21 Negative Blood extract TDp

,::

;lNL:5.66E3tnlz=272.5-273.5 F: - cESI SRM [email protected] [246.fi-247.50,272.50-273.50t MSSpoto1-07021-6040921

fi12.282.8-2U3 Fi - cESI SRM [email protected] [282.75-284.251 MSSpoto1_07021-6040921

NL: 3.2483nvz: 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSpot01_07021'6040921

mfz= 325.t326.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSpoto1_07021 6040921

oo

Ec

€o

.Eo

ffVz= 31 1.5-312.5 F: - cESI SRM [email protected] [311.50-312.501 MSSpoto1_07021 6040921

Time (min)

fo,/+,

C:\Xcalibur\...\Sootl1 07 021 6042017

10(

Y:

EC

ta

7A

65

DU

5C

50

45

40

30

02j16107 04:20:17

NL:2.96E4nlz= 272.1273.5 Fi - cESI SRM [email protected] I246.50-247.50,272.50-273.501 MSSpoto'l_0702 1'504201 7

1.33E4m/z= 246.5-247.5 F: - cESI SRM [email protected] [[email protected] MSSpotol_07021'604201 7

(tlz= 2E2.8-2U.3 F: - cESI SRM [email protected] [282.75-2U.251 MSspotol_07021ir04201 7

NL: 3.74E4r/z= 299.5.300.5 F: - cESI SRM [email protected] [,oa qn-ann qn

325.50.326.501 MSSpotol_07021-6042Ol 7

45

40

Time {minl

&,%( vt)

C:ti(calibuA. \Soot01 070216043106 02116107 04:31:06 Negative Blood extract Tvp

'10(

da

7a

7A

8oo

NL:0ttlz= 272.5-273.5 F: - cESI SRM [email protected] I246.50-247.50,272.s0-273.501 MSSpoto1_0702'1 60431 06

nlz= 246.5-247.5F'. - cESI SRM [email protected] [246.50-247.50.272,50-273.501 MSSpoto1_07021'60431 06

V,lb

nvz= 325.S326.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.501 MSSpoto1_07021'50431 06

oaF

€o

50


(,to)

C:U(calibur\...\S ool01 070216044202 02116107 04:42:02

.riz=272.5-273.5 F: - cESI SRM ms2

1uL EDTA+ C-rn3

u-6c NL: 3.9'1E4

rn/z= 299.$300.5 F: - cESI SRM [email protected] [z9v.JU-JUU.3U,325.50-326.s01 MSSpot01

-07021 -60,14202

NL:4.72E4nrlF 311.5.312.5 F: - cESI SRM [email protected] [311.50-312.501 MSSpoto1_07021'6044202

100-.1I*t

'[email protected]

ms2| 5.00 [

246.fi-247.50,272.50-273.501 MSSpoto1_07021'60/t4202

dz:246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MSSpoto1_07021-6044202

I

o.a66

't0(

9(

8(

7!

nlz= 242.E-2U.3 Fi - cESI SRM [email protected] [282.75-284.251 MSspoto1_07021ii044202

5"w,,

70

5C

35

30

NL:'1.7784rvz= 325.5-326.5 F: - cESI SRM ms23,[email protected] I299.50-300.50,325.50-326.501 MSspot11 _070216044202

( 4os) i

C:U(calibur\...\SpotO1 _07021 6M5255 0?/16107 04:52:55 Negative Blood extract {v(,

90

80

75

70

oc

Etlz= 272.U273.5 Fi - cESI SRM [email protected] [246.5G247.50.272.5c223.s0i MSSpot01_07021'5045255

rlz= 282.V2E'4..3 F: - cESI SRM [email protected] [282.7$2U.251 MSspoto1_0702 1b045255

NL: 2.67E3nvz= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSpoto1_0702 16045255

m/z= 3'11.t312.5 F:- cESI SRM [email protected] [311.50-312.501 MSSpotol-070216045255

oPoE

€oEoo

100

90

85

80

75

70

65

55

JU

45

40

35

JU

a(,+

V46qq)

Time (min)

C:L\calibur\...\Soot01 070216050350 0A16107 05:03:50 5uL EDTA+ A--

-fip

1 00-t

o.-l*l".-l

NL:6.98E4(lz=272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSpoto1-07021 6050350

NL:1.03E4.'].lz= 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50.272.sO-273.501 MSSootol 070216050350

filz= 28?.8-2U.3 F'. - cESI SRM [email protected] [242.75-2U.25t MSSpotol-07021'6050350

qqb

NL: 4.35E4mh= 299.5-300.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSSpot0 l_0702'l 6050350

1.06E4010(

9:

8(

7,

6a

8u

nVF 325.5-326.5 F: - cESI SRM [email protected] I299.50-300.50,325.50-326.501 MSSpot01_07021 6050350

r/z= 311.5-3'12.5 F: - cESI SRM [email protected] [311.50-312.s01 MSSpoto1_07021 6050350

o

o

a

oE


(1

100-.1

I*l''-l

NL:0mlz=246.5-247.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.s01 MSSpoto1_07021'6051444

C:l(calibur\.-.\SpotO1_07021 6051 444 02116107 05:14:44

NL: 4.06E3nllz= 272.*273.5 F: - cESI SRM [email protected] [246.50-247.fi,272.50-273.501 MSSpoto1_07021 6051,144

rnlz= 282.8-2U.3 Fi - cESI SRM [email protected] [282.75-284.251 MSsooto1 07021tt051444

Negative Blood extract lvpNL:2.56E3

Edc

o.z=6

FVz= 299.5-300.5 F: - cESI SRM [email protected].

ms2r5.00 I

299.50-300.50,325.50-326.501 MSSpolo1_07021 605'1444

mtz= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.501 MSSpoto1 _07021'6051 444

r/z= 31 1.5-312.5 F: - cESI SRM [email protected] [311.50-312.501 MSSpotol_07021'6051 444

C:\J(calibur\.,.\SpotO 1 _07021 6052539 02116107 05:25:39 5uL EDTA+ B.-----jb3

NL: 4.47E4nlz= 272.5-2735 F: - cESI SRM ms2291 [email protected] I246.50-247.50,272.50.273.501 MSSpoto1-07021'6052539

NL: 1.03E4ftlz= 246.5-247.5 F: - cESI SRM [email protected] I246.50-247.50,272.50-273.501 MSSpoto1_07021 6052539

mlz= 282.8-2U.3 F'. - cESI SRM [email protected] I282.75-2U.251 MSSooto1 0702'16052539

[, qar-(s"\

NL:4.08E4trVz- 299.$300.5 F: . cESI SRM [email protected] [299.50-300.50,325.50.326.s01 MSSpoto1_0702'1 6052539

n/z= 325.$326.5 F: - cESI SRM [email protected] [299.50.300.50,325.50-326.501 MSSpoto'l_07021 6052539

1001

e5J

no-]I

--leo-l

I

ru-1

'"1^-l*l

p *-l

6.80E4nvz= 31 1.t312.5 F: - cESI SRM [email protected] [311.50-312.501 MSSpotol-0702 1 6052539

Time (min)

C:l(calibuA...\Spot01_07021 6053635

1 001

oJ*l'-l

NL:2.19E3nlz= 272.*273.5 F: - cESI SRM [email protected] [246.50-247.50,272.50.273.501 MSSpoto1_0702 1-6053635

Nz= 282.8-2U.3 F: - cESI SRM [email protected] [282.75-2U.251 MSspot01_07021it053635

Zo't*(sot

0U16107 05:36:35

oc

ooo

Negative Blood extract '.:fr8

- NL:onVr 299.5.300.5 F: - cESt SRM [email protected] I299.50-300.50,325.50.326.501Spoto 1_0702

501 MS121 6053635

1.9583mfz= 325.5.326.5 F: - cESI SRM [email protected] Izw.cu-JUu.tu,325.50-326.501 MSSpolol_07021 6053635

rvz= 311.$3'12.5 F: - cESI SRM [email protected] I311.50.312.501 MSSpot0'1_07021 6053635

C:VcalibuA...\Soot01 07021 60S726

iool "i''u-l I'r-J I

02116107 05:47''26

NL: 4.97E4tvz= 272.*273.5 F: - cESI SRM [email protected] [246.50-247.fi.272.50-273.50i MsSpoto1_07021 6054726

:2.71E9rnlz= 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.s0-273.50] MSSpoto1_07021 6054726

@o

@

@

do

NL:6.88E5nlz= 2E2.E-2U.3 F: - cESI SRM [email protected] I2A2.75-2U.251 MSspot0l_0702'1 i;054726

5uL EDTA+ C 'rvp

NL:6,68E4rvz: 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSpoto1_07021 6054726

NL:6.04E9r/z= 325.5-326.5 F:. cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSpolo1_07021 6054726

7.64E4m/2= 31 1 .5-312.5 F: - cESI SRM ms2a<a n6^r < nn I

311.50-312.501 MSSpot01_0702 1 6054726

10(

9i

8l

7a

d

42

2a

2(

1l

Tlme (min)

C:l'(calibuA...\Spot01_07021 6055824 02116107 05:58:24

NL: 3.66E3mlz=272.5-273.5 F: - cESI SRM [email protected] [246.fi-247.50,272.50-273.501 MSSpoto'l_07021'605582,1

NL:4.15E3mlz= 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.fi,272.50-273.501 MSSpoto l_07021 6055824

44a

Io

o

6

10{

8{

7!

7(

b:

5:

5L

35

3C

=282.+2U3F: - cms2

D15.00 [284.251 MS070216055824

(*')

Negative Blood extract^qjr6

NL:1.07E3rvz= 299.5-300.5 F: . cESI SRM [email protected],325.50-325.501 MSSpot01 _0702'l'6055E24

r/z= 325.5-326.5 F: - cESI SRM [email protected] [299.50-300.s0,325.50-326.501 MSSpoto1 _07021'6055824

NL: 3.1 5E3mfz= 31 1.5.312.5 F: - cESI SRM [email protected] [311.50-312.501 MSSpoto1 _07021'6055824

C:XcalibuA...\SootO1

'ol "it,u'l ll

'o-l I I

02116107 06:09:17 lOuL EDTA+ A llu/'NL: 1.29E5ntlz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.fi,272.s0-273.501 MSSpoto l_07021 606091 7

m/z= 299.t300.5 F: - cESI SRM [email protected] I299.50-300.50,325,50-326.501 MSSpoto1 _07021606091 7

NL: 1.2484nlz= 246.5-247 .5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSpoto l_070216060917

nlz=242.&2U.3 F: - cESI SRM [email protected] [282.75-2U.25) MSSpol01_07021 606091 7

1.66E4ruz= Jl5.+JZb.a f :- cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSpoto1_07021 60609'l 7

o

6E

€o

.!loE.

fo qqb(s4


C:\j(calibur\...\SpotO1_07021 606201 3 02116107 06:20:13

NL:2.74E3fitlz=272.5-273.5 Fi - cESI SRM msz291 [email protected] [246.50-247.50,272.50-273.501 MSSpot01_07021 606201 3

Negative Blood extract TNB

1001

*loo_J

nvz= 299.$.300.5 F: - cESI SRM [email protected] I299.so.5oo.so,'325.50-326.501 MSspoto1_0702'tb062o.t 3

nfz= 31 1.9312.5 F: - cESI SRM [email protected] [311.s0-312.501 MSSpoto1_07021'606201 3

1001

9flI

s0-lqa-l*lroJ

rr-lto-l

es-]

E 60--1

rnlz=246.5.247.5 F: - cESI SRM ms2291 [email protected] [246.50-247.50.272.50-273.soi MsSpotol_07021 606201 3

nlz=282.8-Z8/..X F: - cESI SRM [email protected] [282.75-2U.251 MSSootol 070216062013

L/ tl

ocd

€o

6

Time (min)

(t.t)

C :\Xcalibur\...\SpotO1 _07021 60631 08..,------ 02116107 06:31:08

mlz= 272.5-273.5 F'. - cESI SRM msz' [email protected] [246.50-247.50.272.50-273.s0i MsSpoto1_07021 606310E

NL: '1.03E4

trlz=246.*247.5F:-c

&. +vro( s"r)

1oo-l 'i'"-lil^!il

NL; 8.64E4n/z= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50.325.50-326.501 MSSpoto1_07021'6063 1 O8

1001

qr-.1*tso-l

i

--i80-]

I

tu-]

roloc-1

e .o-l

ESI SRM [email protected] I246.50-247.50,272.50-273.50t MSSooto1 070216063'106

.rJ/z= 242.8-28/..3 F: - cESI SRM [email protected] {2A2.75-2U.251 MSSpoto l_07021 60631 08

C :!Xcalibur\-..\Spot01_0702 1 6064204 02116107 06:42:04 Negative Blood extract -T1)a

r/z= 325.5-326.5 F: - cESI SRM [email protected] [299.5G.300.50,325.50-326.501 MSSpoto1_07021'6064204

100-.]l*l

'I

NL:6.39E3rnlz=272.?273.5F: - cESI SRM [email protected] [246.fi-247.50,272.50-273.501 MSSpoto1_07021'6064204

nlz=246.5-247.5 Fi - cESI SRM [email protected] [246.fi-247.50.272.50-273.501 MSSpoto1_07021 6064204

NL:4.2482ff'lz=282.*2U3F.- cESI SRM [email protected] (

282.75-2U.251 MSSpol01_07021 6064204

o

oE:

do

m/z= 31 1.5-312.5 F: . cESI SRM [email protected] [311,50-312.501 MSSpoto1_07021 6064204

C:LXcalibur\...\Spot01 _0702 1 6065301 02116107 06:53:01 lOuL EDTA+ C

.lj/z=272.5-273.5F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSpoto1-07021'6065301

mlz= 282.*2U.3 F: - cESI SRM [email protected] [282.75-2U.251 MSSpot01-07021-6065301

Oqv

NL: 1.42E5miz= 299.5-300.5 F: - cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSpot01_0702 1 6065301

o.-l*l*-l

*.1I

^-lro-]

ru-l

$ *-1

nz= Jz5.'Jzb.5 F: . cESI SRM [email protected] [299.50-300.50,325.50-326.501 MSSpot01_0702'16065301

(t,")

C:'Xcalibur\...\SootO1 07021 6070351 02116107 07:03:51

r,1z= 272.5-273.5 F: - cESI SRM [email protected]

rl.s2r5.00 [

246.50-247.50.272.50-273.501 MSSpoto1_07021-6070351

ESI SRM [email protected] [246.50-247.50,272.50-273.501 MSSpoto1-07021'6070351

mlz=282.&2U3 Fi - cESI SRM [email protected] [282.7t2U.251 MSsootol 07021b070351


-

ltD6

t*rni.oJ

NL: 1.71 E3rniz= 299.9300.5 F: - cESI SRM [email protected] I299.50-300,s0.325.50-326.501 MSSpoto1_07021 6070351

NL:5.93E3r/z= 325.$326.5 F: - cESI SRM ms234420@15,00 [299.50-300.50,325.50-326.501 MSSpoto 1_07021'607035'l

o

o

4.50E3nvz= 31 L5-31 2.5 F: - cESI SRM [email protected] I311.50.312.s01 MSSpot01_07021 6070351

6" ++(s t,)

i

TM IDIAGNOSTICS

t" 4*ui rz-r)

C:U(uElibur\...\EDTA\BreweA021 507U1 501

t::*lro-l

ru-]

ro-]

tul

^-l6s-1

o ^^ls, ."1

nlz=246.1247,5F: + c 951 Pr', t"[email protected] I125.00.315.00t MS21501

[<. aa'^/ '\*iJruqMA

^ ,,, A"'vV YV\,ry'\,\

( <,t

100 ppm EDTA tm

r#sE RT:0.79 AV: 1


ClXcelibuA...\EDTA\BreweA02 1 307U1 302 0U13107 08:50:58 100 ppm EDTA -l?p

NL: 1.06E5nvz= 299.5-300.5 Ft . cESI SRM [email protected] [299.50-300.50,32s.50-326.501 MS21302

ED'fFronl

oooE:oo6

r/z= 325.t326.5 Fi - cESI SRM [email protected] [299.5G300.50,325.5G326.s01 MS21302

m/z= 311.t312.5 F: - cESI SRM [email protected] MS21302

rnlz=282.E-2U3F: -cESI SRM [email protected] [282.7r2U.251 MS21302

f* ,/r/ o(*\

Time (mrn)

' C :L\calibur\...\EDTA\Brewe rl}ZlzdlUlZ}i\t 0?/1407 02:33:58

rolrul

"-l811

eo-l

'JJ--l

o ^^l"*l

NL:2.87E5fiVz:159.$160.5F:+cESl [email protected] [125.0e315.001 MS21206

NL: 3.71E5Ttc Ms 21206

f*+

NL:5.52E4r.lz=246.*247.5F: + c ESI Full [email protected] [125.00-315.001 MS21206

(<,)

( tOO ppm EDT]) 76.r\----+ c ESI Full ms2 [email protected] [ 125.00-315.00]

\21203 07021209391

\6e

NL:3.39E5mlz= 272.5-273.5 F: - cESI SRM [email protected] [246.50-247.50.272.50-273.501 MS21203 070212093914

L: 1.30E4mlz-- 246.5-247.5 F: - cESI SRM [email protected] [246.50-247.50,272.50-273.501 MS21203_Q7021 209391 4

TIC MS21203_070212A93914

o)oo

_gq)E,

fo ngt(*u\

123 1352,35 2.SB

1472.81

1qTime (min)

% ;:J_^

c:\Xcatibur\..Q{!1-o7o20s0sl 3d}'\ 0?/09107 09:13:09 QsD -fpn

r/z= 159.$160.5 F: +c ESI [email protected] MS20901_o7o2oEo91 309

NL:0fflz= 246.*247.5 F: +c ESI [email protected] [12s.00-31s.001 Ms20901_07020fu9,1309

rnlz= 258.t259.5 F: +c ESI Full [email protected] [125.00.315.00t MS20901_0702orh91 309

!,ooE

o':Eo

r: + cESt rulinilisS.ooqnd.bb iizs.obnri.obf

:3.06E4TIC MS2090 1_070209091 309

4q

Full ms2 [email protected] [ ]2s.00-315.001

trr/z= 157.$'168.5 F: +c ESI Full [email protected] [125.00-315.00t MS2090 1_07020sh91309

({,')

/\C :\XcalibuA...\EDTA\Brewer\02090iw91 02109107 09:17:22 -trF

:,1

NL:5.65E5nr/z= 159.S1605F: + c ESI Full [email protected] [125.00-315.001 MS20902

li:,lz=246.+247.5F: + c ESI Full [email protected] MS20902

:3.81E4

:3.47E3

:4.57E5Tlc MS 20902

rn/z= 167.$168.5F: + c ESI Full ms2305,[email protected] [125.00-315.001 MS20902

rrz= 258.5-259.5F: + c ESI Full [email protected] [125.00-315.001 MS20902

Eo

:ooGE

oo

o

Go

f,*u{

100-l

qnl--l.ol.^l:^.1*-l--.1

( srt)

C:\Xt]alibuA...\EDTA\BreweAO2090700903 J 0209107 09:25:27 (sss onm each EDrA, d12 EDTA )U., -.) J 9f

'::l-.]

NLr 4.38E5nVz= 159.5-'160.5F: i c ESI Full [email protected] [125.00-315.001 MS20903

rnlz=246.*247.5F: + c ESI Full [email protected] [125.00-315.001 MS20903

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REFERENCES

to+,to(<^+)

Joumal of Analytical Toxicology, Vol, 21, November/December I 997

1

r

L

t:1f1ttliq

The Analysis of EDTA in Dried Bloodstains byElectrospray LC-MS-MS and lon Chromatography-

Mark [. Millerl, Bruce R. McCordl, Roger Martz2, and Bruce Budowlet.tForensic Science Research and Training Center, FBI Labotatory, Quantico, Vrginia 22135 and zChemistryIoxicology L)nit,FBI Laboratory, Washington, D.C. 20535

blood that behave as catalysts and/or cofactors,EDTA-preserved blood tubes use the salt forms of EDTA:

Analytical methods were developed to determine the presence of the disodium, dipotassium, or tripotassium salt, The con-ethylenediaminetetnacetic acid'(EDTA) in dried bloodsrains ro centration of EDTA in its free acid form in a drawn bloodprovide probative information when allegations of evidence tube is 1000-2000 mg/L (ppm), depending on the volume oftanpering have been made in criminal cases. A simple screening blood and the capacity of the tube. The free acid and saltmethod using ion chromato6nphy to analyze slains was found to forms are all water soluble at this concentration. EDTA isbe quantitative to lhe 5 ppm level. The presence ofEDTA was stable on storage and on boiling in aqueous solutions, butthen confirmed usingnegative and positive ion mode tiquid it does decarboiylate when heatel to temperatures of l!g"Cchmmatography-tandem mass spectrometry (LC-[tsMS) .. (I). lt is an excellent comprexing agent and forms water-

ff*ttl|ii,*ill*T"L'$:|,ofi"1:"T[li?,"'il:o't '.ilui,ir',r.tes with neaity auieavy metars. Thererore,

preservative EDTA. one intensting observalion in these ns'ults aqleous exhactions of dried bloodstains should readity iso-

was the adsorption and postanalysi-s release of EDTA i" il;-'- late^E-DTA in solution.

chromatograpiic system. In order to avoid cros contamination . IDTA is used as a chelating agent in a variety of mate-of samplei resulting from this phenomem, it was found to bc rials, and several chromatographic methods have beennec€ssary to use EDTA-free blood extracls as btanks in the developed for its determination. A number of the methods[C-MS analysis of bloodstains. employ reversed-phase ion-pair liquid chromatography (LC)

for analysis of EDTA in foodstuffs (2,3), water (4,5), radio-active waste (6), and pharmaceuticals (7), Gas chromato-rntroduction i:ill[Jr,?Lffiflj.,,:'J,ffi[i$:1?",:""f1,.1ffi1;(lC) is an additional logical approach for the analysis of

The collection of blood at crime scenes and for legal pro- EDTA (6). All of the previously mentioned LC methods useceedings is a common practice used to inculpate or excul- ultraviolet detectors and lack the specificity of liquid chro-pate individuals associated with evidentiary blood at crime matography-mass spectrometry {LC-MS). An additionalscenes. Allegations of "planting" blood evidence from col- level ofselectivity in the analysis of EDTA can be added bylected reference specimens has occurred in some criminat the use of LC-MS-MS. A simple extraction technique cou-investigaiions, and this issue may be resolved by the deter- pled with positive ion and negltive ion LC-M$-MS methodsmination of exogenous components that would not ordi- was developed for the analysis of EDTA in preserved driednarily be present in authentic crime scene evidence. bloodstains. Pneumatically assisted electrospray (ES) wasEthylenediaminetetraacetic acid (EDTA, also known as used to ionize the chromatographic efflueni before massedetic acid,. C 1eH16N20s, molecular weight,292.24) (Figure spectnl analysis of the charged species. A secondary methodl), a chemical commonly added to collected blood speci- using ion chromatography was devetoped to provide a quan-mens, can be used to implicate the origin of a dried blood- titative presumptive test for the presence of EDTA as will asstain as coming from this type of preserved specimen tube. corroborate the results of the LC-lvlS-MS analysis. In aThe purpose of the EDTA in the tube is to prevent coagu- blind trial conducted on 42 bloodstains using it', rimlation and enzymatic degradation by chelating metals in lhe extraction protocol for IC and LC-MS-MS;problems_occurredintheLC-Iv1S-Iv1Sanalysis.Subsequently,allll;.1?::iil:Ttr'#1,'::::Hil1::,ffi:iffff,#f"T9,,, refined extraction method was developeo ror rb_usjr,riatdincluiondcndimptyendffi€rnbythcFcdart Burcauoltru€nisarim. - analySiS Of dfigd blOOd.

4"1 44bReproduoion (photocopyint) of edito{ial ."(.ff,r?),"a1 is prohibired wirhout pubtisher's permission.

;xperimental*

ChemicalsAmerican Chemical Society reagent-grade ammonium

hydroxide, disodium EDTd cupric sulfate, and high-perfor.mance liquid chromatography (HPLC)-grade acetonitrile werepurchased from Sigma Chemical (St. Louis, M0), HplO-grademethanol was obtained from EM Science (Cibbsto,vn, NJ).Certified sulfuric acid (2.5M) and sterile Vacutainer blood tubeswithout additives (red top)and with EDTA (K3) (lavender top)were obtained from Fisher Scientific (Fairlawn, NJ). Nanopurewater from a Barnstead (Dubuque, IA) water purificationsystem was used for sampla and mobile phases. The deuteratedstandard of EDTA-dp (Figure 1) was purchased from Cam-bridge Isotope Laboratories (Andover, MA).

Instrumentation

Ion chromatographic analysis was carried out using a Waters510 HPLC pump (Milford, MA) coupled to a Hamilton (Reno,

$UtgRAlg0#Lchromatoeraphic column, sample detec-ruon was perrormed us'fi'g; bpectroflow-273 tunableabsorbance detector (Kratos Analytical Instruments, West-wood, NJ.) Instnrment control and signal procasingwere per.formed using a Millenium 2010 chromatography manager(Waten, Milford, MA), Additional ion chromatographic analyses'lere performed using a Waters 600 analytical HPLC coupled to

Waters 990 photodiode array detector.The LC-MS-MS work was performed on a Hewlett-Packard

(Palo Alto, CA) HP 1090 ternary LC with autosampler con.nected to a Finnigan MAI (San Josd, CA) TSQ 700 triple*tagequadrupole MS using a Finnigan electrospray interface. Argonwas used as a collision gas for MS-MS. The instrument was setup to scan the mass nnge in 0.5-2 s. A flow rate of 0.3 mUminwas used on a Hamilton (Reno, M PRP-I polymeric column(2.1 x 150 mm).

Procedure

Test samples were made by drawing whole blood sam-ples into unpreserved and EDTA-containing tubes, Thebloodstains were prepared on the same day by applyingbetween 2 and 50 pL ofunpreserved or EDTA-containingblood onto sterile cotton Iinen. Additional sarnples wereprepared using liquid whole blood from a laboratoryvolunteer.

loumal ofAnalytical Toxicology, Vol. 21, November/December 1997

. For the initial study, 25 to 5096 of the stained area (up t0tl2 cm2l was cut out of the cotton swatch. The cutting waiplaced,in 50 or 100'pL of 0,02SM copper (il) sulfate(enough

.to _cover sample). The samples were soaked insolution for 3 or more hours before vortex mixing and cen-trifuging at 3000-9000 rpm for l0 min. After passing thegmqle through a 0.2-pm nylon syringe filter, injections oi25 pL were made for lC analysis, The IC mobile phase was3mM sulfuric acid/methanot (g5:5). The flow rate was2 mUmin with a detector wavelength of 25{ nm. This wave.length was. subsequently changed following analysis by aUV photodiode array detector that indicatea fne pea[absorbance maximum for the copper/EDTA complex occursat 243 nm. Following IC, the residual copper extract sam-ples were diluted with 25 pL ofwater and l-pl injectionswere made for positive ion LC-MS-MS. This preparationmethod was used for all IC analyses and for thi initial runby LC-MS-MS of the 42 blind trial samples. SubsequenrLC-MS-MS analysis samples were prepared by the proce_dure given in the next paragraph.

A different extraction procedure wai*developed forLC-IIS-MS analysis to eliminate copper (ll) sulfate, whichcaused arcing problems in the electrospray interface, from theextnct. This procedure was used t0 prepare samples for bothnegative and positive ion LC-MS-MS but not IC analpis. Aportion (up to l/2 cm2) of the bloodstain was extracted bvinserting the sample into Millipore (Bedford, I'4A) Ljltrafree-Micentrifugal filters made of a polysulfone membnne (typePTTK) with a nominal molecularweight cutoff of 30,000 DiLtons. AIter the addition of 25 pL of water, the sample wasallowed to sit at room temperature for 45 min. The filter tubeswere centrifuged for approximately l0 min, and the filtntewas collected for analysis.

Positive ion LC-MS-MS data were collected by scanning forproduct ions of (M + H)+ at 293 u from 12&296 u at a collisionoffset of-20 V The interface was set for a spray voltage of4 kV,

a sheath gas pressure of 90 psi, and an auxiliary gis flow of5 units. The interface capillary was maintained at 200"C. A

mobile phase of acetonitrile and water (S:95) with 0.06%ammonium hydroxide was used.

Negative ion LC*MS-MS data were acquired by scanningfor the 300 u product ion from the iron adduct of UOtl at344 u. A scan window of 29&302 u was emptoyed. The col-lision offset for selected reaction monitorin{ of the 44 u

mass loss was 20 V The interface was ieT6r aiptay voltage

1 lournal of Analy

'Results and

lt*i A revlew 0lE .,:. grapnlc appro

,,lC analysis ot

" copper or iror

'this analysis

llsample deriva

E

o56

t0

r 6.5E

acoc

of 4.5 kV a sheath gas pressure of 50 psi, andan auxiliary gas flow of 5 units. The heatedcapillary was set for 200"C. The optimized-column mobile phase for negative ion wasfound to be acetonitrile and water (80:20) with0.03% ammonium hydroxide.

The isotopic pattern calculation was per-formed on the ChemPuter from the Departmentof Chemistry at the University of Sheffield,Sheffield, Englandt, The experimental isotopepattern was calculated by adding six scanstogether and the same number of backgroundscans were subtracted to obtain the result.

5.5

Fi6'ure 2. loE0TA-preset

Figure 1. Structures, formulae, and molecular weights for EDTA and EDTAdl2,

'Thf w€b .ddr6r for tfE Chefipuler is hnp.//ffi,sh€{&.uw-chcny'cfrmplrcrtElop6.hht, tJtlb

rr/Decemberof Analytica I Toxicology, Vol. 2 1, Novemlrer/December I 997

ts and Discussioned area.rtting

)s A review of the litenture indicated that ttre best chromato- I l- -rt J ',04 approach for the determination of EDTA used HPLC or

nng andi analysis of colored complexa formed between EDTA andor iron (2-6). Although procedures uist for performing

ile phase

ow rate

analysis by GC, thae methods rcquire time-consumingle derivatization and are prone to matrix interferenca (3).

n. Thisanalysis

ed theusing the ion exchange column PRP X-100 with sulfuric

nplexextract

tL iniprepar

re initialSu

Y the

veloped

rlfate,

.rce, from:les for

:xtracted

brane

nt applications published by Hamilton indicated accept-separations of EMA+opper complexes could be canied

acid/methanol mobile phases (8). Initial IC tating with Wdetection was carried out on standard samples of S0-100 ppmEDTA disolved in 0.025M copper (lI) sulfate. The results withthis eluent system were encounging; therefon, further testswere carid out on samples of liquid blood. IC samples were pre-pared from 200 pL of whole blood (EDTA preserved) by fintdiluting il to 2 mL with water and then diluting *re solution l:lwith 0.05M copper (ll) zulhte. This prepantionwas centrifugedfor 7 min, which left a clear supernahnt with a brown preripi-tate at the bottom. A large orcas of copper (II) sulfate helped toensure conversion of all free EDIA to the copper complet The

r passing

injection

^" 400

'le

If{llii{w"i&l

":,$t'1

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'scannfEDTAl. Thethe 44

ry vol) psi,

re hea

'timiion

;20) ';20)witBdil

.vas pei,!

rartmer{:effieldisotonr{

500,000

400,000

F 300'000oo

200,000

100,000

00.2 4.4 0.6 0.8 1 1.2 1.4

Time (mln)

500,000

400,000

.B 300'0006g

2o0,oo0

100,000

Tlme (mln)

Figure 3. EDTA analysis of the proton adduct ion rnlz 293 by positive ion

full scan LC-MS-MS. Reconstructed ion chromatogram (solid line, scan

range 128-296 u) and EDTA product ion rnlz 160 (dashed line) traces

from unpreserved (A) and EDTA-preseved (8) blood stain extracts,

0 0.2 0.4 0.6 0.8 I 1.2 1.402468

Iime (mln)

Figurc 2. lon chromatograms of a 50 ppm EDTA standard (A) and anEDTAareserved blood extracl (B) at a detection wavelength of 254 nm.

scaru:

result of this analysis is shown in Figure 2. Similar analyses

using FeCl3 and Fe2(S04)3 to complex with EDTA did not preduce precipibtes and showed large interfering peal$. fu a resulfall further tests were performed using Cu(lI) sulfate at a con-centraiion of 0.025M in each sample. In a set of serial dilutionsin water; the analysis wu shown to have a linear nnge from zeroto greater than 500 ppm EDTA with a minimum detectablequantity of 5 ppm EDTA for the injected sample.

,lourna I of Ana lytica I Toxicology, Vol. 2 t, November/December I 997

A Hamilton PRP-I column was used to sepante EDTA for MSdetection in order to reduce interference from other comlpounds in the blood. Other blood components were retarded onthe column and minimized peak overlap with EDTA whichhas a short retention time. IC mobile and stationary phaseswere not used for the MS procedure because of the strongbuffer ion concentrations required for ion exchange that led ioelechical arcs in the electrospray interface. An additionar reason

IEaaEOU0,

.go-l840E

100

80

20

130 150 170 190 210 230 250mh

Figure 4. Positive ion LC-MIMS product spctrum from collision-induced dissociation of EDTA ion (M+H)+ at n/zzg3.

OOiliiHoC-cq\.H /cft-'bon

?N-c'.h-o-rr-Ni __+'of"* .,t-,1o"

o m/2p93 0

I

I

fo

"t\ t"u)LoEN-clt-clt-N\ * HqCH

Hoc.c/ tcq-coH

ll lo m/z 247 o

H /ct+z-o$co + cFl=61;-'\*-.o,-il

ny'z1\2 o

otl

HOC-CFtz\

N-H " CFh./noc-ct{/

tlo

rn/z 160

I

I

t

Figure 5. Fra8rnents observed by collision-induced dissociation "€tt^f^{€"ucr ion (m/2293) in posirive ion LCrvlMS analysis of EDTA, T

preserved blood. /( gty\' f:i::)'.

11"',r:,;

l:ttt.)*:,ffi

l6urnil of Analytical Toxicology, Vol. 2l , November/December I 997

. for keeping the ionic shength of the mobile phxe minimized is

I higher ion concentrations may suppress analyte ionization (g).,i Standard sample solutions (10-100 ppm) of disodium EDTA

i in water yielded abundant adduct ions by electrospray sample

:, loop injection (flow injection analysis, FIA) or Li-ltS in inepositive ion mode. However, analysa of disodium EDTA withor without chromatography gave variable spectra as a result of

;:, the formation of numerous metal complues with EDTA The' DDTA adduct ion (lvl + H)+ at mlz 293 was observed even' though the mobile phase was alkaline. Other charged species

observed in standard sample solutions and their proposed

identities were as follows: mlz 3I5, (M + Na).; m/23!7,(M -2H+dlttt;-. mlz 337 , (M - H + ZNal+; mlz 346, (M - 2H +Fettt)+; mlz 368, (M - 3H + Felll + Na )*; and mlz jgl, (M - 4H+ Feill + 2Na)*. The electrospny interface is constructed ofstainless steel and aluminum and accounts for the presence ofFelil and Allll complexes in analysa of disodium EDTA. Theelectrolytic nature of electrospray has been shown to formiron complexes from the stainles steel spny needle (10).

Negative ion FIA-MS (sample loop injection)or LGMS gen-

ented several ions with sampla of disodium EDTA including(l'l-H)- at mlz 29I and the doubly charged ion (M - 2H;-z utmlz 145. Adduct ions were also observed in negative ion modewith the same metals (pstll and Alllt) as pbsitive ion mode.Complexed species indicated from FIA-MS or LC-MS and theirproposed identities were: mlz 313, (M - 2H + Nah m/z 315,(M - 4H + Alrr)- mlz 335, (M - 3H + 2Na)-; and mlz 3M,(M - 4H + Fer)-. The negative ion spectra were also poorlyreproducible in the relative intensity of the various ions forsiandard runs ofdisodium EDTA,

Positive ion LC-MS was also oramined using a series of mix-tures of acetonitrile and 0.06% ammonium hydroxide. Themobile phue (5:95) was selected as it gave the best responseand consistency for 0DTA analysis. This mobile phase gave(M + H). ions atmlz293 for the disodium EDTA standard (10to 100 ppm) and was the base peak for EDTA in preservedblood samples, No prominent fragment ions were observed inthe spectrum of EDTA, and thus it was necessary to analyzesamples by LC-M$-MS to obtain structunlly significant ionsfor identification (Figure 3), In the blood samples, no inter-ferences were found in the reconstructed ion (RIC) tnce for theMS-MS of ion 293. MS-MS of the 293 ion generated threeproduct ions with a base peak at 160 u and two smaller ions at

masses 132 nd247 u (Figure 4). The three-product ions (132,

160, 247) and their associated losses are coruistent with theknown EDTA{12 spectrum which has product ions at mlz 140,168, and 259, respectively (Figure 5). The neutral losses cor.respond to carbon monoxide, a di-carboxylic acid secondaryamine, and formic acid.

A blind trialof the analysis procedura was performed inde-pendently by IC and by positive ion LC-MS-I"1S. Forty-twodried bloodstain extncts prepared for IC analysis were analyzedin the blind study to determine if BDTA preserved btood couldbe distinguished from unpreserved blood spots. Although thesamples were diluted with 25 pL of water before LC_MS_MS,some electrical arcs still occurred in the elecbospray interfacebecause of the copper (ll) sulfate in the samplej. Tire volumeof the original bloodstain samples ranged from 2 to 50 pL.Although all stains containing EDTA (n = 2l) were correctlvidentified using the IC technique, LC-MS-Mscorrectly deter-mined 20 of the 2l positive samples, Both techniques cor-rectly identified all of the negative samples (n = Zli. A stainsample that gave a positive result in the IC test had indicationsof DDTA by the LC-MS-MS procedure but was considered tooweak to be called positive on a single resull This was an extractof half of the smallest EDTA blood spot (2 pL) in the 42 sam.ples (i.e., approximately t UL). At the time of the testing allother positives gave significant area counts (several hundredthousand) for the 160 u product ion, and both 132 and 24? uions were present. The false-negative result lnd an area countof 80,000 for ion 160, and both other product ions were pre-sent. A conservative decision was made to interpret the sampteas negative until further testing could be completed.

A revised extraction method was dewloped for LC-MS-MSafter the initial testing to eliminate the cupric sulfate-inducedarcing problerns in the interface and to obtain more concen-trated sample extracts. A simple procedure was devised toextract the stains in centrifugal filters after a A5-min soakingin water. A molecular weight cutoff of 30,000 Da was chosen toremove particulate matter, blood cells, and large proteins fromthe filtrate while still maintaining an adequate flow throughthe filter disc, A retest by positive ion mode LC-MS-MS ofseveral dried stains (preserved and unpresennd btood spots)produced positive results for all of the EDTA containing bloodwith area counts ofseveral hundred thousand for the 160 ionand negative results for all unpreserved spots. The sample

that previously had been deemed a negative(2-trL EDTA blood spot) gave an area count of1,000,000 for ion 160 by the revised method.'iboof the positive sampies were extnctd a secondtime, and it was found that, on average, 9l% ofthe EDTA response (peak area for 160 production) was in the first extract.

In the negative ion mode, the ferric ion com-plex with EDTAatmlz344, (M -4H * p.rrl)-, c0n-sistently appeared in analyses of the disodiumEDTA standard and was the base peak for EDTA inpreserved blood samples. The identity of the 344ion wu verified by comparing the calculated iso-topic formula for (C1jH12N206Fe) with experi-mental data (Table I). No prominent structural

Table l. Calculated and Experimenlal tntensity (%) of the Molecular lonCluster (CrgHr2N2OsFe) for the lron Complex with EDTA (M - lH+Fettt;-Observed by Negative lon LC-M$-i4S for an EDTA Standard

n/z Predicled intensity Experimental intensity

342

343

344

J{)

346

JqI

348

6,3

0.8

f00

2.9

U.J

U

6.4

2.1

t001t,

/.. I

u,o

0.2

u4b( szo

peaks were observed in the LC-MS spectrum of this complex,

MS-MS of the 344 ion gave a strong signal for the product ion

atrnlz 300 (M - C02f. A second LC-MS-MS method, in neg-

ative ion mode, was developed to screen for the presence ofEDTA in bloodstains by observing the mass-toclnrge ratiotnnsition from 344 to 300 in the selected reaction moniiorinfmode (SRM). This method of MS-MS operation is selective

-1L

Journal of Analy,tical Toxicology, Vol. 21 , November/December I 997

and sensitive because the instrument scaru over a limited mass

range while measuring a specific trarsition resulting frorncollision-induced dissociation. The MS-MS ion tnce of rnlz300 and the RIC show no extnneous signals other than themajor peak for the EDTA derived species from blood extracti(Figure 6). Some lmown (n = 4) and unknown (n = 2) blood

samples were successfully tested as a trial of the negative ionmethod.

A comparison of negative ion and positive ion LC-MS-MS of

a blood stain revealed an 80-fold difference in intensity ofEDTA signal for the 160 ion (positive) over the 300 ion (nega.

tive). Because of [he use of MS-MS in both techniques,responses from other components in the blood were notobserved, and, therefore, boih analyses were deemed selectiveThe positive ion mode is a better means of confirmationbecause there are three structurally significant product iorucompared with only one for the negative ion mode.

The IC, negative ion and positive ion LC-MS-MS methodswere used on investigative case samples (n = 9) to determine ilevidentiary crime scene blood might have been tampered evi-

dence. A phenolphtlulein-presumptive test for blood ( 1l ) wapositive on all testd stains (n = 4). In addition, all extncts of

the stains appeared red in color as supportive evidence for the

praence of blood. All three techniques were negative for EDTA ;

in the bloodstains. Howarer, in the positive ion SRM (mlz tnw a,

sition 293 to 160) LC-MS-MS analysis of one of the stairu.

from a sock, a small peak appeared with the correct retentiontime for EDTA" IC and negative ion results did not indicatr

EDIA in the sample and positive ion full scan LC-MS-MScould not confirm all three EDTA product ions from the parent

ion at 293 u. In known EDTA samples, the three techniqueshad consistently agreed, and intersities were strong enough for

ihe known samples to confirm the three product ions by

MS-MS of the parent ion at 293 u. A potential criticism of the

evaluation of the results is the inabilig to determine the exact

quantity of blood in a sample. In these studies, it was found that

sample sizes as small as I pL of blood generated more than adrquate signal for EDTA. A sample of this size would leave a

dried blood spot of 0.1 cm2 on a swatch of cotton linen.A study wu conducted to determine if the small uncon-

firmed signalobserved in the case sample could result froma

carry-over in the system. An EDTA-dt2 standard was used fot

this work to prevent interference from endogenous levelsof

EDTA After sevenlinjections of ttre EDTA-drz standard (500

ppm), blank samples of different substances were run. No

signal by LC-I'IS-MS was observed after a single injection dblanls such as water, mobile phue, or salt solutions. Howevet,

injection of EDTA free blood extrach, following a blank injec'

tion, gave a response for the EDTA-d12 compound tha[,

decreased with each repetition (Figure 7). The low signal in ti8icase mentioned above was likely a result of an interferendresulting from the previously injecterl standard. It is theoiril'that, when a blank blood matrix is injected onto the s.vstefn,

residualEDTA adsorbed onto sita in the column and hrbintisreleased by competing metal ions in the blood extract. There'

fore, it is recommended that the only suitable blank after injr;tioru of EDTA is EDTA-free blood extncl Multiple injections ot

EDTA-free blood extract should be made uniii no observablqt

10,000

8000

6000

4000

2000

04.2 0.4

Time (min)

10,000

8000

6000

4000

2000

01.2

Fi8ure 6. EDTA analysis of the iron addud ion at ndz344 by negative ion

SRM LC-MtMS. Reconstrucled ion chromatogram (solid line, scan range

297-JO2 u) ard EDTA product ion r/z 100 (dashed line) traces from

unpreservd (A) and tDTA-presewed (B) blood sain exrfacts.

/r-: \::,:1,

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purnal of Analytical Toxicology, Vol. 21, November/December 1997

EDTA peak is detected before any case samples are anatyzed bthis method.

EDTA is an additive in a variety of foods, such as pickla,

canned mushrooms, and salad dresings, and potentially could

occur in human blood at low lewls. However, in a study of

radio-labeled EDTA" ingated samples were found to be elimi-

nated mainly by excretion with minimalgastrointestinal tract

absorption (12). Thus, it is unlikely that measurable quantities

would be found in the blood by the employed techniques,

Attempts to measure EDTA in unpreserved blood by the use of

samples up to I mL in volume were negative. A search of the

literature did not find any measurements of EDTA in blood

from dietary consumption levels.

Another concem in the analysis ofbloodstains is the stability

of EDTA in the dried spots after extended periods of storage.

Samples of EDTA preserved bloodstains (n = 2) were analyzed

after 2 yean of storage at room temperature. LC-MS-MSanalysis of the additive-free samples were negative and the

preserved samples were positive for EDTA"

Conclusion

Methods described herein demonstnte the abili$ to deter-

mine if tampering of bloodstains may have occurred using

EDTA-preserved blood The coupling of a quantitative tech-

nique with the specificity of the LC-MS-MS procedures is apowerful analytial protocol. Specific procedures were devel-

oped to identifu and control the effect of matrix interference on

the umples. MaFix interference can be minimized by injecting

EDTAlree blood artncts before the analysis of any samples.

The accuracy ofthe determination was supported through the

use of simulated investigative case samples. Experiments on

aged, dried blood indicate it is possible to determine EDTA in

stains after at least 2 years of storage.

Acknowledgments

The authors would like to acknowledge the assistance of

Kelly Hargadon lvtount Jill Smerick, Kathleen Keys, Barban

Koons, Tim Mchughlin, John Paulson, Dean Fetterolf, and

Robert Mothershead, II.

References

M. Windholz, Ed. The Merck /ndex. Merck & Co., Rahway, Nl,'1976, p 463.

,1, De Jon8, A. Van Polanen, and J,J.M. Oriessen. Determination of

ethylenediaminetekaacetic acid and its salts in canned mush-

rooms by revased-phase ion-pair liquid chromatography. /. Chromatogt.553i 243-48 (1 991).

C. Retho and L. Diep. Low-level determination of ethylenedi-aminetetraacetic acid in complex matiices. Z, Lebensm Unters

Forsch. 188: 223-26 (l 989).

B. Nowack, F.C. Kari, S.U. Hilger, and L.Sigg. Determination o{

dissolved and adsorbed EDTA species in water and sediments by

HPLC, Anal. Chen. 68:561-66 (1 996).

P.J.M. Eergers and A.C. De Croot. The analysis of EDTA in water

by HPLC, Wat Res.28:639-42 (1994).

M. Unger, E. Mainka, and W, Konig. Quantitative determinationof EDTA and its behavior in radioactive waste solutions using

HPLC. Fresenius J. Anal. Chem.329: 50-54 (1 987).

1,

2.

c

6.

0.2 0.4 0.6 0.8 1 1.2 1.4

Time (min)

0 0.2 0.4 0.6 0.8 1 1.2 1.4

nme (min)

Figure 7. Sample carry over experiment to demonstrate the matrix effecl

of blood extracts. The top chart (A) is an injection of mobile phase after

tire injections of 500 ppm EDTAdl2 standard. The chart on the bottom (8)

shows the results of injecting an extract from a non-EDTA-preserved

blod tube after the blank analysis in (A). EDTA-d12 analysis of the proton

adducl ion n/z 305 W positive ion iull scan LC-M!MS, Reconstructed

ton chromatogram (solid line) and EDTAdl2 product ion r/z 1 68 (dashed

itne) traces,

4L/b

E,L. Inhan, R.L. Clemens, and I'A. Olsen. Determination of

EDTA in vancomycin by liquid chromatography with absorbance

ratioing for peak identification. J. Pharm. BioM. AnaL S (6):

513-20 (1990).

Hamilton application note #286,287.

P. Kebarle and L. Tang. From ions in solution to ions in the gas

ohase, Anal. Chern. 55(22)1 9724-86A (1 993).

C.f. tjames, R.C Dutky, and H.M. Fales. lron carboxylate oxygen-triangle complexes detected during electrospray use of organicacid modifien with a comment on the Finnigan TSQ'70 elec'trospray inlet system. /. Arn. Soc. Mass Spec, 5: I 226-31 (l 995).

Journal of Analytical Toxicology, Vol. 21, November/Decemhr 1997

ll, W,C. Eckert and S.H. lames. lnterytetation of Blodstain Evi.dence at Crime Scenes. CRC Press, Ann Arbor, Ml, 1993, p 120.

12. H. Foreman and T.T. Trujillo. The metabolism of raC labeldethylenediaminetetraacetic acid in human beings, /, Lab. Clin,Med.43;566-71 (1954).

Manuscript received January 31, 1997;revision received Aoril 29, 1997.

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AC 8197: Determining EDTA in Blood

Analytical ChemistrY

August l, L997

Analytical Chemistry 1991,69, 477 A-480L'

Copyright @ lggi by the American Chemical Society'

Page I of6

Determining EDTA in Bloodb

Amurdertrialshedslightontheneedforabetteranalyticalmethod

Robjn-,L-,-$he-p,pardJaskH-enion

Cornell UniversitY

It is not often that a story on the national evening news uses words such as "liquid chromatography" and

,,mass spectrometry'i"Ai"iyti";l chemists who lieard such reports.during the murder tnalrhe state of

carifurnia v. orentharT"riiiii^pson immediately perked up their ears, amazed that the analytical

J.tuits of FBI laboratory testing were actually making headlines'

The subject of the testing was EDTA (ethylenediaminetetraacetic acid) issue was whether police had

,,planted,, or tampereJ *Ttn Utooa evidencl in an attempt to shore up the case against Simpson' The

possibre outcomes "r,r,. i"Jirg were simple: Either EbTA-was present or it wasn't. Qualitative testing

began (i), but as is usually the iase, l:lfrllg is that simple. There was eYidence of some EDTA, at levels

much lower than in;DTi-;r"served bloodl The questions "How much EDTA is there?" and "Are the

detected levels "orrririrnt

with'normal' levels or those that would result from tainted blood collected in

E iA anticoagulant blood tubes?" arose immediately.

The lead prosecutor, Marcia Clark, tried her best to present this scientific evidence. But how do you

convince a jury or.itir.", that knows little about analytical chemistry that the EDTA came not from a

lavender-stoppered lrrt. u,rt from a bleeding o.J. Simpson? Althoug! i!.mav not have been the only

weak point in the prosecution's case, it certiinly *ur u factor in the trial's outcome. Because of this

criminal case, determining EDTA in human blood has become a topic of renewed interest'

what was wrong with the laboratory testing? First, it was not clear whether the method had ever been

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AC8197 Determining EDTA in Blood Page 2 of 6

used before. Most likely the method was developed quickly under a great deal of time pressure. In

,etrorpe"t, FBI chemisti now believe that the EDTA detected may have been injection carryover in the

lCnfSnrnS (2) instrumentation because a water blank instead of a matrix blank had been run before the

*-pf. Se.oni, the EDTA concentration was not rigorously quantitated, Cert-ainly, the volume of the

blood stain could have been estimated. EDTA is present at about 4.5 mM (-1300 ppm) in EDTA-

preserued blood, which would be a very concentrated sample and easily detected by electrospray

LC1MS/I\4S. It appeared that the amount of EDTA detected in the forensic blood samples was orders of

magnltuae below 4.5 mM. Regardless of what happened in the Simpson trial, it became apparent that a

definitive and valid method foi determining EDTA in human blood was needed.

EDTA I}ASTCS

EDTA is a metal-complexing agent that has been popular since its commercialization in the early 1950s

i-rj. rr* free-acid structure *itrr u molecular weight of 292.1 is shown in Figure 1a, and a three-

dimensional representation of EDTA complexed with nickel(Il) with a molecular weight of 347.0 is

shown in Figure lb. EDTA has four acidii protons t!{ are sequentially ionized at solution pH values of

2I,2.67,6.i6, and lo.z6,respectively ({. The disodium salt is commonly used as an anticoagulant (5)'

and the familiar lavender-stoppered biood collection tubes contain enough EDTA to give a final

concentration of - 4.5 mM. Uion mixing with blood, the EDTA immediately chelates the available

calcium. Because calcium is necessary for the formation of fibrin, coagulation cannot take place (5).

dor ,*S*oru&z'4't{O-i-*

Figure 1. (a) EDTA's free-acid structure and (b) three-dimensional structure of Ni-EDTA'

EDTA is also used extensively as a food preservative, a water-softening agent, and to deliver trace

minerals in animal feeds (e. bespite its ubiquitous presence, metabolism studies have shown that little,

if any, EDTA should be present in human blood. In 1954, a metabolism study using laco-lubel.d

calcium-EDTA given intravenously showed that EDTA was detectable in the plasma but not in the

blood cells ( Z). 6r, u,u"rug e, 95o/o of an oral dose was recovered in the urine and feces within three days

of administration with no EDTA detected in the plasma, and the remaining 57o was detected in the urine

within 1g h. More recent metabolism studies using the NaFe(III)-EDTA complex report that it

dissociates during digestion and confirm that only about 5% of the EDTA is absorbed and excreted in

urine (8).

DETERMINING EDTA IN BLOOD AND PLASMA

Although there are numerous published methods fo).a.t"t-ining EDTA in various matrices such as

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AC 8197: Determining EDTA in Blood Page 3 of6

mayonnaise (9), wastewater (/0), and ophthalmic solutions (11), our lab and one other group have

reclntly attempied to develop improved methods that could be used for the forensic measurement of

EDTA in biological matrices (12, 13).

There are numerous ways to prepare samples containing free or chelated EDTA. The first and most

obvious is no sample pieparation at all. If the pH of the sample is not adjusted and if metal

contamination can be eliminated, the natural distribution of EDTA and its metal chelates can be

determined. This is not the most sensitive approach because the EDTA signal would be distributed

among several different metal species or peaks. In addition,.quantitation would be difficult because any

chang-e in the sample matrix could change the complex equilibria. Therefore, all the methods used to

*""r-ur" EDTA itielf focus on preparing a singular EDTA-containing peak or compound.

For GC, the analyte must be reasonably volatile and thermally stable. Because EDTA is not volatile, it is

usually derivatized by esterifying the four carboxyl groups with methanol, butanol, or isopropyl aicohol

(13-l i). This liquid-iiquid extraction is a labor-intensive, multistep procedure that is difficult to

automate. For L-C or capillary electrophoresis (CE), the most logical way to convert all available EDTA

to a single compound is to aOA an exCess of one metal that strongly complexes with EDTA. Although

iron(Illj and copper(Il) are commonly used (,11, 16),we found that nickel(Il) complexes with EDTA just

u. "if.rtiu"ty,

anA iihas several advantages: Heating is not required, the complex is stable down to

pH\t3, and the complex gives a higher signal by ion spray MS than either the iron or copper complexes.

DEVELOPING A CE/MS/MS METHOD

Several reports in which CE was used to determine metals using EDTA as a.complexing reagent have

been published in the literature (17, /8). Using these reports as a starting point, we predicted that an

"MS-hendly" CE separation could be developed that would minimize the chemical additives introduced

into the mass sPectrometer.

The intricacy of interfacing the capillary to a mass spectrometer is the reason the technique is considered

nonroutine. Although many qualitative CEA{S applications have been reported, very few quantitative

methods have been described in the literature (19,20). Therefore, we used this opportunity to achieve

two goals: to offer an improved technique for measuring E-DTA in biological matrices and to

deminstrate that CE/MS can be used in a routine manner for quantitative bioanalytical applications.

Although MS may not be the most sensitive CE detector available, it offers a high level of selectivity as

well asaider appiicability than, for example, laser-induced fluorescence (21). For example, the full-scan

CEI11{S separation shown in Figure 2a displays the EDTA dishibuted as five different metal complexes.

Figure 2b shows the same EDTA standard in which the predominant ion m/2347, caused by Ni-EDTA,

ha! been extracted from the total ion current data. This type of selectivity can be exploited by using the

selected ion monitoring mode in which only the ion(s) of interest would be detected.

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Figure 2. (a) Full-scan GE/IVIS electropherogram of five EDTA-metal chelates and (b) extracted ion electropherogram

of Ni-EDTA.

Additional selectivity can be achieved using MS/TvIS by selecting a precursor ion that is characteristic of

the analyte, fragmenling it into one or more ions, and selectively detecting on€ specific fragment from

the selected prJcurso. i6n. For example, a full-scan single mass spectrum of the Ni-EDTA complex in

Figure 3a shows the deprotonated molecular anion at m/z 347, which corresponds to the [Ni2+"H+

,gbre4-]- ion. This precursor ion may be fragmented using collision-ind1cgd dissociation within the

.econd-quadrupole region of a triple-quadrupole mass spectrometer. The full-scan product ion mass

;;;il; from the fralmentation-of m/z 347-inFigure 3b shows product ions m/z 329 and 257, which

are characteristic of the Ni-EDTA complex'

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Figure 3. (a) Fult-scan mass spectrum and (b) full-scan product ion scan of Ni-EDTA'

This additional selectivity can be put to use in the selected reaction m-onitoring ISnfuO mode by

monitoring only the rpr.ifi.d traniition m/z 347 fragmenting to 3.29.l"t*:=fctivity is achieved via

the initial LE separation, which gives a characteristic migration time for Ni-EDTA. It is highly unlikely

that a chemical compound otherihan Ni-EDTA would result in this characteristic transition at the

specifred migration iime under the described experimental conditions'

To illustrate this point, blank and Ni-EDTA-spiked p!a9m1 samples were simply diluted with water'

filtered, and analyzed 6y CE with tIV detection and CE with SRM detection. The blank plasma in

Figur. '4a

andthe t-pvrNi-EDTA-spiked plasma in Figure_4b are indistinguishable by CE/W because

ofrn. excessive chemical background detected at200 nm. In contrast, when analyzed by SRM-CE^VIS'

the same blank plasma sample i-s free of all matrix peaks (Figure 4c); whereas the Ni-EDTA-spiked

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AC 8197 Determining EDTA in Blood

plasma displays only the targeted Ni-EDTA peak (Figure 4d).

of using tandem MS for this type of targeted analysis.

This example clearly

Page 5 of6

shows the advantage

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Figure 4. UV detection versus SRM detection.

CEruV analysis of (a) blank plasma and (b) Ni-EDTA-spiked plasma. SRM-CEA4S analysis from m/z 347 to 329 of (c)

blank plasma and (d) Ni-EDTA-spiked plasma.

To further minimize the possibility of interference, we developed an automated anion-exchange solid-

phase extraction procedure. The complete SRM-CEA4S procedure uses 100 pL of plasma, to which is

added 50 ng of 113C0;EDTA internal standard, brought to pH 9-10 with ammonium hydroxide, and

complexed using nickel nitrate. The sample is diluted 1:45 with 0.05% formic acid (pH 3) and then

extracted using itrong anion-exchange solid-phase extraction media. The sample is eluted, evaporated,

and reconstituied in 30 pL of water. The extract is injected for 0.1 min at 950 mbar inlet pressure onto a

50 pm X 60 crn amine-coated capillary. The separation is performed using a CE running buffer of 30

*M u--onium formate atpH 3 (adjusted with formic acid) and -30 kV with 50-mbar inlet pressure

throughout the run. A homemade self-aligning liquid junction CEA4S interface is used with a makeup

liquiJof 5 mM ammonium formate in95o/o methanol at lOpl/min(22,23). Atriple-quadrupole mass

splctrometer is used in the negative-ion mode with SRM of the transitions m/z 347-329 for Ni-EDTA

and m/z 35 1-333 for the internal standard Ni-(13C4)EDTA. The complete method and validation are

described in this issue in reference24,

Using this sample preparation procedure and the SRM-CE/\4S method, we achieved a detection limit of7.3 n:glmL EDiA in human plasma and a lower level of quantitation (LLQ) of 15 ng/ml (-6 frnol

iniecled). If this method waJused to determine whether a forensic blood stain had been "planted", this

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2t912007

AC 8197: Determining EDTA in Blood Page 6 of6

LLQ conesponds to "planting" 1-3 nL of EDTA-preserved blood. Because it would be physically

difficult to manipulate such a small volume, any such forensic sample would probably contain at least I

pL. This hypothetical scenario illustrates the excellent sensitivity and potential forensic usefulness of the

method. Similarly, the GCilvIS/I4S method developed by Ballard and colleagues demonstrated a

comparable detection limit of 10 ng/sample, which corresponds to -7 or 8 nL of EDTA-preserved blood

(13).

CONCLT-ISIONS

Many techniques have been used over the years to determine EDTA in various matrices, and most can

be adapted to biological samples. Howevet, SRM-CEA4S provides the highest specificity and the best

detection level of any method currently published. .

We have been able to demonstrate that typical human plasma samples do contain detectable EDTA, but

at levels that are lower than the LLQ reported in this work. The LLQ of our method, at 15 ng/ml, is a

factor of 105 lower than the typical concentration found in EDTA-preserved blood (4.5 mM or 1.3 X 106

ng/ml.). But more importantly, we have demonstrated that CE/lvIS methods can be used for routine

bioanalytical analysis with acceptable precision, accuracy, and adequate detection levels for quantitation

of trace-level concentrations (24).

CE/MS techniques will undoubtedly become an important forensic technique because of the low

volumes of sample required for analysis, as well as the ability to use the mass spectrometer to achieve

selectivity higher than with any other on-line detector.

The question of blood-evidence tampering in a oriminal trial has led not only to improved analytical

techniques for the determination of EDTA, but also to the demonstration that a relatively new technique

is ready to be used as credible scientific evidence in the courtroom.

REFERENCES

tF ChemCent"t m Pubs Div. I'lome Page

Copyright @ 1997 by the American Chemical Society.

q(bhttn' //nrrhs. acs.ors/ho tartcll acl 97laug/det.html (s;r) 2t9t2007

n

:?:H:fff#Insrumert Opcrattoo g SunniLs2:.b;:

Issue Date: 0621/06

l:;lfl;3

Performance Monitoring Protocol (QA/QC)for the Finnigan LCQ LClMS @Sf)

1 Scope

This document addresses the performance monitoring (QA/QC) of the Finnigan LCQ LC/MS

system consisting of a Finnigan LCQ MS and a Waters LC. It is an analytical instrument used to

11nalyzea wide u*i.ty of evidence and must be maintained in such away as to verify its

reproducibility from analysis to analysis and its reliability in court.

2 Principle

The LCe system is comprised of a Waters Liquid Cluomatograph (LC) and a Finnigan ion trap

LCe Mass Spectrometei (VfS). The instrument is configured with an API source that is capable

of Uotn electrospray (ESI) and atnospheric pressure chemical (APCI) ionization. The

instrument is primariiy used in ESI mode. However, this protocol can also be used for APCI

provided the method of ionization is clearly labeled in the resulting data and documentation.

befinitions and guidelines for following this protocol are outlined in the "General lnstrument

Maintenance PolicY."

3 EquipmenUMaterials/Reagents

a. lnstrumentation - Finnigan LCQ MS, API Source, Waters Alliance 269012695 LC,

and Data System with XCalibur software (or equivalent)

b. API Gas - Nitrogen, 99.99% (high purity or equivalent)

c. Ion Trap Gas - Helium,99.99yo (high purity or equivalent)

Methanol, HPLC grade

Deionized Water, 18 M(.l Milli-Q or equivalent

Acetonitrile, HPLC grade

Acetic Acid, reagent grade


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l:;:tr3

h. Ulftamark 1621 (Finnigan or equivalent)

i. Caffeine (Sigrna or equivalent)

j. MRFA (L-methionyl-arginyl-phenylalanyl-alanine acetate) (Finnigan or equivalent)

k. Ammonium Hydroxide (NruOD, reagent grcde

l. Codeine (Sigma or equivalent)

m. Brucine (Sigma or equivalent)

n. Reserpine (Sigma or equivalent)

o. Volumetric glassware

p. Infusion Syringe - 10 to 500 pL LC syringe (Hamilton or equivalent)


4.1 Testmix

The Testrnix is used to assess daily operating performance, mass assignment, and continued

integrity of the system. To prepare, weigh 5.0 mg caffeine, 1.0 mg codeine, 1.0 mg brucine, and

1.0 mg reserpine into a 100-mL volumetric flask. Bring to the mark with methanol and mix well.

Store the solution in the refrigerator. It has a shelf-life of three years. This preparation may be

appropriately scaled up.

4.2 Cahbrttion Solution

The calibration solution is used for coarse tuning and calibrating the mass spectrometer over the

entire mass range. This procedure only needs to be performed when the instrument has been

moved, down for a long period of time, undergone a major repair, or warranted based on system

performance.

The calibration solution is a solution of caffeine, MRFA, and Ulhamark 1621 in

acetonitrile:methanol:water containing l% acetic acid. To prepare this solution, follow the

procedure in the LCQ 'Getting Started' manual. Store the solution in the refrigerator. It has a

shelf-life of three years. This preparation may be appropriately scaled up.


fn q*,-( s+")

FBI LaboraoryChemistry Unit

Insrument Operation & Support SubunitInst 202-0.doc

Issue Date: 06nl/06Revision: 0

Pase 3 of 8

5 Calibration

The calibration procedure should be performed as needed, when the instrument has been moved,down for a long period of time, undergone a major repair, or warranted based on systemperformance.

a. Load a 250 pL syringe with the calibration solution.

b. Using capillary tubing, connect the infusion syringe to the ESI probe assembly, andplace in the syringe pump.

c. Set the syringe pump to the correct syringe type and set the pump rate tol0pl/minute.

d. Load the tune file "ESI TLTNE" (or equivalent).

e. Check that instrument is in POSITIVE ION mode and collecting CENTROID data.

f. Set the detector using the parameters listed in the 'Instrumental Conditions' section ofthis protocol.

g. Turn on the syringe pump and verifu that the solution is flowing out the ESI needle.

h. Engage the ESI probe and turn on the MS.

i. In Tune Plus, open the Calibrate dialog box, choose the'Automatic'tab and check theindividual tests or'Select All' and then 'Start.'

j. When the calibration is complete, it will display whether or not the calibration wassuccessful.

o If the procedure fails, repeat the calibration.. When the procedure passes, print the report and evaluate the calibration

solution spectrum using the 'Decision Criteria' section of this protocol. If theresults are acceptable, print the spectrum of the calibration solution.

k. If all requirements are within specification, prepnre the documentation as outlined inthe "General Instrument Maintenance Policy." If any requirements fail, the IOSS

This is an uncontrolled copy of a controlled documenl

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H:#ltr"f#Insu,ment Operatt"" U r

"*:to!:oblillIssue Date: 06/21106

lil:'lr3Manager will determine the corrective action to be taken.

6 Sampling

Not applicable.

7 Procedures

7.1 Daily Checks

The following steps are to be performed daily. Enter the appropriate information in the QA/QClog for tracking purposes.

a. Record the remaining disk space on the hard drive. Use Windows Explorer program(WindowsNT) to verify that the hard disk has at least 100 MB of free disk space. Donot use if less than 100 MB remain.

Record the line pressure of the building nifrogen supply (API gas). The regulatorshould read between 60 and 100 p.s.i. If it cannot maintain this pressure, contactIOSS. If the nitrogen'is supplied by a gas cylinder, record the tank pressure. changethe tank if less than 100 p.s.i. remaining.

Record the line pressure of the building helium supply (ion trap gas). The regulatorshould read between 30 and 60 p.s.i. If it cannot maintain this pressure, contactIoss. If the helium is supplied by a gas cylinder, record the tank pressure. changethe tank if less than 100 p.s.i. remaining.

Check the Ion Gauge to ensure that no significant leaks are present in the system. Donot use if the pressure is higher than I x 10* torr.

Prepare the instrument for analysis of Testnix. Verify that the instrument has theconect source probe installed (ESI), the correct tune file loaded (esi_tune orequivalent), positive ion mode selected, and centroid data being collected. If acolumn is installed, remove it from that system and replace it with the infusioncapillary tube.Perform an analysis of the Testnix prior to the analysis of evidence using parameterslisted in the'Instrumental Conditions'section of this protocol. Start the HPLC pump.Engage the ESI probe and turn on the MS. Start an acquisition using a filename such


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c.

d.

FBI Laboraiory

rnstnrment operati"" o rififf Hff llInst 202-0.doc

Issue Date: 06nll06

lilii:i3

as 'testmix' (or equivalent). Make three 5 pL injections of the Testnix solutionapproximately 10 seconds apart by using the manual loop injector, and then stop thedata collection. Evaluate the results using the 'Decision Criteria' section of thisprotocol. If the results are acceptable, print the TIC and spectra for all components inthe Tesrnix.

g. If all requirements are within specification, prepare the documentation as outlined inthe "General lnstrument Maintenance Policy." If any requirements fail, contactIOSS.

7.2 As Needed Checks

a. Re-cut or replace the sample capillary as needed.

b. Clean or replace the heated capillary as needed.


Refer to the "General Instument Maintenance Policy" for procedures on minor deviations.

8.1 Testmix

Liquid ChromatoeraphMobile Phase:

Flow Rate:Column:lnj Volume:Number of Inj:


95:5 methanol:water + 0.03% ammonium hydroxide0.2 ml/minNone5pL

aJ

ESIesi_tuneFull Scan100-650 miz


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Insrument Operation & Support SubunitInst 2024.doc

Issue Date: 06nl/06Revision: 0page 6 of 8

8.2 Calibration


9 Decision Criteria

ESIesi_tuneFull Scan100-2000 mlz

9.1 Testmix

Verify the results of the Tesftnix. The following ions should be observed in the three Testrnixinjections:

. Caffeine I95 mlz

. Codeine 300 mlzo Brucine 395 mlzr Reserpine 609 mlz

9.2 Calibration

Veri$ the results of the calibration. The calibration will indicate if the procedure wassuccessful. The individual ions for the calibration solution are:

r Caffeiner MRFAr Ultramark

L95 mlz524 mlz1022m/zIl22 mlzL222mJz1322m/z1422 mlz1522 m/z1622 mlz1722 mlz1822 mlzL922 mlz

greater than 5%greater than 50%greater than 5o/o

greater than2DYogreater than 50%greater than 50%greater than 80%greater than 50%greater than 50%greater 'han 20o/o

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Eo q,/,(sv+)

FBI laboratory

Instrument operatt"" & s:lof,t'HbYJ l:Inst 202-0.doc

Issue Date: 06/21/06Revision: 0Page 7 of 8

10 Calculations

Not applicable.


Not applicable.

12 Limitations

Only properly trained personnel shall perform duties involved in the operation, maintenance, ortroubleshooting of this instrument.

13 Safety

Take standard precautions for the handling of all chemicals, reagents, and standards. Refer tothe FBI Laboratory Sof"ty Manual for the proper handling and disposal of all chemicals.Personal protective equipment should be used when handling any chemical and when performingany t)?e of analysis. Many instrument components are held at temperatures of 250oC andhigher. Precautions should be taken to prevent the contact of skin with heated surfaces andareas.

14 References

Manufacturer's lnsfument Manuals for the specific models and accessories used.

"General Instrument Maintenance Policy" (Inst 001) Instrument Operation and Support SubunitSOP Manual.

"Liquid Chromatograph General Maintenance Protocol" (Inst 003) Instrument Operation andSupport Subunit SOP Manual.

"Mass Spectrometer General Maintenance Protocol" (Inst 004) Instrument Operation andSupport Subunit SOP Manual.

FBI Laboratory Safety Manual.


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To: Madeline A. Montgohory, Marc A. LeBeautr'rom: Cynthia L. Morris-Kukoski uLDate: February 26,2007Subject: Competency EDTA

Madeline Montgomery successfully completed her competency test for the EDTA inBloodstains SOP. She 100% correctly identified which blood samples contained EDTA andwhich ones did not.

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t

competnrcytest

Date: 212012007

To: LEBEAU, MARC A. (LD) (FBD

From: Jay A. Clark ,5['

RE: Competency Test

Congratulations, you have successfully completed your competency exam for the Analysis of EDTA

in Blood Stains.

Please see the attached Key for the correct answers, and the procedure for the preparation of the test

samnles.

€v'/4u(u"4

competnrcytestkey

Date: 211512007

RE: Competency Test Key

Competency Tests for Analysis of EDTA in Blood Stains results are as follows

JCI - non-preserved blood

JC2 - EDTA preserved blood



JQJ:- norypreserved blood

JC6'- EDTA preserved blood.':JC7 - noir:preserved blood

t:

J :cB

t n*-Pteserved blood

JC9 - EDTA preserved blood:l''"rl r

ldt0 - non-preserved blood

Prepared Yy, (htT.}la'h--

fn qqL

Date: 1- t5-07

(t *)

Preparation of Competency Tests for "Analysis of EDTA in Blood Stains" SOP:

1. Seiect a sterile cotton-tip swab and label it with a unique identifier.

Z. Place l0 pL of blood @DTA-preserved or non-EDTA-preserved) onto the cotton

tip swab. Document if the swab was prepared with blood containing EDTA.

3. Repeat with appropriate number of swabs.

4, Allow all swabs to dry overnight. Blindly distibute to test participants.

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Detailed Qualifications and Proficiency Test Report for JASON D BREWER 0731'0000

Controlled Substance

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81412005 12:00:00AM

Drug Analysis

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Sample Prep.,Wet Chem. & Inst. Analysis

Expiration Date without a new PT QualTypeLinklD

912312007 11:59:58PM 000000000000223

Identifier 05'15C

Staff Position

Test Source External

Source Unit

Other Comments CTS 05-502 saUsfactory completion

Supplier Collaborative Testing Services

Preparer Name

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LT-PTPM Notificauon of Test 9/8/2005 12:00:00AM

LD-PTPM Review NoUfied

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8/1U2005 12:00:00AM

912312005 11:59:59PM

91812005 12:00:00AM

LtlLl2005 12:00:00AM

'entifier 06-17D

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B/10/2006 12:00r00AM

912212006 11:59:59PM

91t212006 12:00:00AM

L2l5lZ006 12:00:00AM

Supplier Collaborative Testjng Services

PreDarer Name

Verifler Name

Validator Name

LT-PTPM Notification of Tesf. 911212006 12:00:00AM

LD-P|PM Review NoUfied


LD-PTPM Eval

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Fage L of 1

Deta!!ed Qual$flcatiosls amd Froficie T"est ReportDate: 212812007

Report Descripticn:\TU Personnel use this

Trace Analysis (Chem.)

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to view detailed

Bank Dyes

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Sample Prep.,Wet Ctrem. & Inst. Analysis

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IdentiRer 05-16C

Staff Position

Test Source Intemal

Source Unit Chemistry

Other Comments Test set #4- satisfactory completion

Supplier

Preparer Name Deborah Wang

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slL8l2006613012006

sl3Ll2006I

12:00:00AM

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12:00;00AM

12:00:00AM

Supplier

Preparer Name Pamela Reynolds

Verifler Name Eileen Waninger

Validator Name Jason Brewer

LT-ffPM Noufication of Test 5/31/2006LD-ffPM Review NotiRed


LD-PTPM Eval

qlb

l2:00;0OAM

( n'4Paae t of 1

Deta!led {,saIlfications and Fnoficiency Test ReportDare: 212812007

?,eport Description:TU Personnel use this to view detailed test for selected staff.

Toxicology

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QuanUtaUve - Drug Analysis

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QualTypeLinkID

000000000000739

Detailed Qualifications and Proficiency Test Repoft for MARC A LEBEAU 0781-0000

Identifier 05-58

Staff Position


Source Unit

Other Comments FTC-A- satisfactoy completion

Distribution Date 3/!71?oo5 12:00:00AMDue Date SI5IZOOS 11:59:59pMPT Complete Date SF12OO5 12:00:00AMTestee Feedback 8/5/2005 12:00:00AM

Supplier College of American pathologists

Preoarer Name

Verifier Name

Validator Name

LT-PTPM Notification of Test 5/5/2005 12:00:00AMLD-PTPM Review Notified

UC Designee Frinal Eval

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rntifier 06-38

-.aff Position

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Source Unlt

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311612006 12:00:00AM

5/812006 11:59:59PM

5/312006 12:00:00AM

612012006 12:00:00AM

Supplier College of American Pathologisb

Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification of Te'i'. 51312006 12:00:00AMLD-PTPM Review Notified


LD-PTPM Eval

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Detalled ualiiications and Froficlen Test ReportDate: 212812007

Q.eport DescriptionrATU Personnel use this to view detailed and test for selected staff.

Detailed Qualifications and Proficiency Test Repo* for MARC A LEBEAU 0731-0000

Toxicology

QualificaUons Date

tlLlI999 12:00:00AM

Quantitative - Drug Analysis

Most Recent Proficiensy Test

413012002 11:59:59PM

Complete Examination & Analysis


LLl5l2004 11:59:59PM 000000000000275

Identifier 99-18A

Staff Position SUPERVISORY CHEMIST-UNIT CHIEF

Test Source Extemal


Other Comments

Distribution Date

Due Date

PT Complete Date

Supplier CAP

Preparer Name

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Validator Name

LT-mM Noufication of Test 5/1/2000 12:00:00AM



rntifier 00-17

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Test Source Extemal

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Testee Feedback

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Due Date

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LIlLlt999 12:00:00AM

L2lL6lL999 12:00:00AM

l2ltllL999 12:00:00AM

ltlL6l2000 12:00;00AM

L2lZLl2000 11:59:59PM

1212612000 12:00:00AM

5/712001 12:00:00AM

8lL3l200L 12:00:00AM

91251200L 12:00:00AM

91251200L 12:00:00AM

t2l3t/200t 12:00:00AM

Testee Feedback 5/3/2000 12:00:00AM LD-PTPM Eval

Supplier College of American PathologisE

Preparer Name

Verifier Name

Validator Name

LT-mM Noufication of Test 51217001 12:00:00AM

LD-FI?M Review Notified


LD.MM EVaI

Supplier CAP

Preparer Name

Verifier Name

Validator Name

LT-ffiM NoUfication of Test 12731/2001 12:00:00AMLD-mM Review Notified LZl3tlZ}}L 12:00:00AM

UC Desisnee Final Eval 1213112001 12:00:00AMLD-PTPM Eval

Identifier 01-15


Test Source Extemal


Other Comments

IdenUfier 02-2



'rce Unit

Supplier College of American Pathologists

Preparer Name

Verifier Name

Validator Name

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Setailed Qua$ifications and Froficiency Test R ort*ate: 217812007

qeport Description:ATU Personnel use this to view detailed test for selected staff.

Detailed Qualifications and Profrciency Test Report for MARC A LEBEAU 0781-0000

31L812002 12;00:00AM

413012002 11:59:59PM

413012002 12:00:00AM

71L612002 12:00:00AM

of Test 71L612002 12:00:00AMDue Date

PT Complete Date

Testee Feedback

LD-PTPM Review Notified


LD.PTPM EvaI

Identifier 03-27A



Source Unit

Other Comments See attached memos


Preparer Name

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Validator Name

LT-PTPM NoUfi cation of Test 1/15/2004 12:00:00AMLD.PTPM Review NoUfied


LD-PTPM Eval

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Testee Feedback

L012712003 12:00:00AM

LLl712003 11:59:59PM

t2l9lZ003 12:00:00AM

L012004 12:00:00AM

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Setalled Qualifications and F Test Report

test for selected staff.

Oate; 212812007

aepo* *escription;iTU Personnel use this lo view detailed

Toxicology

Qualifications Date

L/t/L999 12:00:00AM

QualitaUve - Drug Analysis


Interprebuon of Results

Expiration Date without a new PT QuaffypeLinklD

519/2007 11:59:5BPM 000000000000738

Detailed Qualifications and Proficiency Test Report for MARC A LEBEAU 0731-0000

Identifier 05-58

Staff Position


Source Unlt

Other Comments FTC-A- satisfactory compleUon

Distribution Date 3fl7lzOOS 12:00:00AMDue Date SfinOOS 11:59:59pMPT Complete Date SF?OOS 12;00;00AMTestee Feedback Bl5l2OOS t2:00:00AM

Supplier College of American PathologisE

Preparer Name

Verifier Name

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LT-PTPM Notification of Test 5/5/2005 12:00:00AMLD-PTPM Review Notified


LD-PTPM Eval

ntifier 06-38

-aff Position


Source Unit

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Testee Feedback

12:00:00AM

11:59:59PM

i2:00:00AM

12:00:0OAM

3/t612006

sl8l2oo5513/2006


Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification of Test 5/3/2006 12:00:00AMLD-FIPM Review Notified


LD-PTPM Eval

vlb( u,,)

Page ,. of 1

Setailed nralificatiosrs and FrofEclency Test ReportDate; 212812007

R.eport Description:ATU Personnel use this to view detailed ualifications and test for selected staff.


Toxicology

Qualifications Date

LltlL999 12:00:00AM

Qualibative - Drug Analysis


413012002 11:59:59PM

Complete Examination &,Analysis

Expiration Date without a new PT Qual[ypeLinklD

Lt/512004 11:59:59PM 000000000000274

Identifier 994Staff Position SUPERVISORY CHEMIST-UNIT CHIEF



Supplier CAP

Preparer Name

Verifier Name

Validator Name

LT-mM Notificauon of feC(. 31L711999 12:00:00AM

LD-PIPM Review Notifled 7lt3lt999 12:00:00AM

UC Desisnee FinalEval 8/10/1999 12:00:00AMLD-PTPM Eval 3/15i2000 12:00:00AM

Supplier CAP

Preparer Name

Verifler Name

Valldator Name

LT-PTPM Notification of Test 8/30/2000 12:00:00AM

LD-PTPM Review Notified 8/30/2000 12:00:00AM

Uc Deslgnee Final Eval 812912000 12:00:00AMLD.PTPM EVaI

'entifier 00-6

rff Position SUPERVISORY CHEMIST-UNIT CHIEF

Test Source Elternal


Other CommenE

Distribution Date

Due Date

PT Complete Date

Testee Feedback

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

3lL7/t999 12:00:00AM

31291t999 12;00:00AM

71211999 12:00:00AM

81411999 12:00:00AM

61712000 12:00:00AM

61t912000 12:00:00AM

6ltgl2010 12;00:00AM

8/30/2000 12:00:00AM

8/13/2001 12:00:00AM

9125/?00t 12:00:00AM

9lZ5l200L 12:00:00AM

L2/3U200L 12:00:00AM

Identifier 01-15




Supplier CAP

Preoarer Name

Verifier Name

Validator Name

LT-PTPM Notification of Test 1213U2001 12;00:00AMLD-PTPM Review Notified Lzl3tl200t 12:00:00AM

UC Desisnee FinalEval 1213112001 12:00:00AMLD-PTPM Eval


Preparer Name

Verifler Name

Validator Name

IdenUfier 02-24

Staff Position SUPERVIS0RY CHEMIST-UNIT CHIEF

Test Source External'''Jrce

Unit

5o q,/U( 1,,,

-rher Comments

Detailed Qaratriflcatissts and Fg'oficiency Test Re*ate:, 212812007

'eport Description:\TU Personnel use this to view detailed qualifications and test for selected staff.

Detailed Qualifications and Proficiency Test Report for MARC A LEBEAU 0731-0000

DistribuUon

Due Date

PT Complete Date

Testee Feedback

3lt9l2002 12:00:00AM

413012002 11:59:59PM

4/3012002 12:00:00AM

71t612002 12:00:00AM

LT-ffiM Notification of 7lt6lZ002 12:00:00AMLD-ffiM Review NoUfied


LD-PTPM Eval

Identifier 03-27A



Source Unit


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LD-PTPM Eval

Other Commenb

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See attached memos

t012712003 12:00:00AM

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LZl9l2003 12:00:00AM

2/1012004 12:00:00AM

C / /,Cv Vlb/\( utal

Fnoe 2 nf 2

S-etailed Quallfications and Froflclenr T'est RepoftDate: 2128120Q7

Repoff DescriptionlATU Personnel use this to view detailed oualifications and test for selected staff.


Toxicology

Qualifications Date

L/t12004 12:00:00AM

Blood Alcohol


Interpretation of Resulb

Expiration Date wlthout a new PT QuaflypeLinklD

IdenUfier 05-27A

Staff Position


Source Unit

Other Comments CAP AL1-C- satisfactory completion

Distribution Date

Due Date

PT Complete Date

Testee Feedback

91212007 11:59:58PM 000000000000736

Supplier College of American PathologisB

Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification of Test 10/1412005 12:00:00AM

LD-F|PM Review Notified


LD-PTPM EVaI

'rntifier 06-14A

,ff Position


Source Unit

Other Comments

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Due Date

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Identifier 06-13A

Staff Position


Source Unit

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10i5l2005 12:00:00AM

L012012005 t1:59:59PM

t011412005 12:00:00AM

L21t212005 12:00:00AM

61t912006 12:00:00AM

613012006 11:59:59PM

712112006 12:00:00AM

91t12006 11:59:59PM

712112006 12:00:00AM


Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification of Test



LD.PTPM EvaI

Supplier Quality Forenics

Preparer Name

Verifier Name

Validator Name

LT-PrPM Notification of Telr. 7FI:Z006 12:00:00AM

LD-PTPM Review Notifled


LD-PTPM EVaI

Y /,cv VVb/'\( {zrs7Paqe L df 1

Setailed ualificaticns andDate: 2lZBIZOOT

Q.eport Descriptionl\TU Personnel use this to.Jlgw detailed ualifications and

Test R

Lest for selected staff.


Expiration Date witfrout a new pT QualTypeLinklD

@Toxicology

Qualifications Date

t/t/L999 12;00:00AM

Detailed euafifications and proficiency Test Report

Blood Alcohol

Most Recent proficiency Test

L0/20/2004 12:00;00AM

for MARC A LEBEAU 0731-0000

L0/20/20C4 11:S9:S9PM 000000000000272

Other Comments

Distribution Date

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PT Complete DateTestee Feedback

Other Commenb

Distribution DateDue Date


IdenUfier

Staff Position

Test Source

Source Unit

Other Comments

Distribution DateDue Date


IdentifierStaff Position

Test Source,rce Unit

6/1511999 12:00:00AM6/2s11999 12:00:00AM6/2211999 12:00:00AM8/4/1999 12;00:00AM

Supplier CApPreparer Name

Verifier Name

Validator Name

LT-PTPM NoUfi cation of TestLD-PTPM Review NoUfiedUC Designee Final EvalLD.PTPM Eval

6/15/1999 12;00:00AM6/24/1999 12:00;00AM8/10/1999 12:00:00AM

Identifier 9g-7Staff PosiUon SUPERVISORY CHEMIST_UNIT CHIEFTest Source ExternalSource Unit Chemistry Unit

'ntifier 00-12,ff Position SUPERVISORY CHEMIST-UNIT CHIEF

Test Source ExternalSource Unit

3/15/2000 12:00:00AM

Supplier College of American pathologistsPreparer Name

Verifler Name

Validator Name

LT-PTPM Noufication of TestLD-PIPM Review NotifiedUC Designee Final EvalLD-PTPM Eval

t2/4/2000 12;00:00AM

9/1912000

9/2912000

9/2912000

L2/18/2000

12;00:0OAM

11:59:59pM

12;00:00AM

12:00:00AM

01-164

SUPERVISORY CHEMIST.UNIT CHIEFExternal

Chemistry Unit

Supplier CApPreparer Name

Verifier Name

Validator Name

LT.PTPM Nouficauon of TestLD-PTPM Review NoUfiedUC Designee Final EvalLD-PTPM Eval

9/t81200t9/27/200t9/241200t

2/18/2002

12:00:0oAM

12:00:0OAM

12:00:0OAM

12:00:0OAM

2/18/20022/18/20022t6t2002

12:00:0oAM

12:00:0OAM

12:00:00AM

02-188

SUPERVISORY CHEMIST-UNTT CHIEFExternal

Supplier College of American pathologis8Preparer Name

Verifier Name

Validator Name

5o,(a

vLner Comments

iletailed Quallfications and Fnofic T'est ReDate: 212812007

teport Description;ATU Personnel use this to view detailed test for selected staff.

Detailed Qualifications and Proficiency Test Report for MAR.C A LEBEAU 0731-0000

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t0lt9l2002 12:00:00PM

t0/2512002 11:59:58PM

1012512002 11:00:00AM

tU26/2002 12:00:00AM

LT-ffiM Notification of 1012512002 11:00:00AMLD-PTPM Review NoUfied


LD-PTPM EvaI

Identifier 03-25A



Source Unit

Supplier College of American pathologisb

PreDarer Name

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LT-PTPM Notification of Test t0/2112003 12:00:00AMLD-PTPM Review NoUfied


LD-PTPM Eval

Other Comments

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Due Date

PT Complete Date

Testee Feedback

10/15/2003 12:00:00AM

t012812003 11:59:59PM

1012t12003 12:00:00AM

Lt/24/2003 12:00:00AM

{* u+e,( o,)

Paqe 2 of ?

Setailed Qerafrlfications asld Ps's$iclency Test Repoft*ate: 212812007

Repo* DescrlptionlATU Personnel use this to view detailed and test for selected staff,

Detailed Qualifications and Proficiency Test R.eport for MARC A LEBEAU 0731-0000


Qualifications Date

L/r/t999 12:00:00AM

Drug Analysis


Complete ExaminaUon & Analysis

Expiration Date without a new PT QualTypeLinkID

000000000000224

Identifier 99-5A


Test Source Extemal

Source Unit Chemistry Unlt

Supplier CTS

Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification oF Test



LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

5/18/1999 12;00:00AM

7181t999 12:00:00AM

7lUL999 12:00:00AM

8141t999 12r00:00AM

7lL3lL999 12:00:00AM

ilt31t999 12:00:00AM

8/10/1999 12:00:00AM3/15/2000 12100:00AM

':ntifier 00-38

"aff Position SUPERVISORY CHEMIST-UNIT CHIEF



Supplier CTS

Preparer Name

Verifier Name

Validator Name

LT-PTPM NoUfi cation of Test



LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

51312000 12:00:00AM

612812000 12:00:00AM

611312000 12:00:00AM

817/2000 12:00:00AM

81712000 12:00:00AM

8/712000 12:00:00AM

712812000 12:00:00AM

{o qqu( r'd

Page 1 a{ L

Detalled Qwalificatiosrs and F*atet 2/2812007

{epoft Sescription;\TU Personnel use this to view detailed qualifications and legt for selected staff.

iletailed Qualifications and Froficienry Test Report for MARC A LE8EAU 0yBt-000O

Trace Analysis (Chem,)

Qualifications Date

LltlL999 12:00:00AM

Bank Dyes

Most Recent Profi ciency Test


Expiration Date wi$rout a new pT QualTypeLinklD

t21612002 11:59:59pM 000000000000261

Identifier 99-38

Staff Position SUPERVISORY CHEMIST-UNIT CHIEFTest Source Internal


Supplier

Preparer Name Waninger, Eileen MarieVerifier Name

Validator Name

LT-PTPM Notifi cauon of TeSt Sl L7 / 1999 12:00:00AMLD-PTPM Review Notified Sn7/Lggg 12:00:00AMUC Designee Finat Evat 5/4/1ggg 12:00:00AMLD-PTPM Eval 31IS/ZOOO 12:00:00AM

Oher Comments

Distribution Date

Due Date

PT Complete Date

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3lt6lL999 12:00:00AM

41271t999 12:00:00AM

4/t91L999 12:00:00AM

41271L999 12;00:00AM

&,/qa,r'r,l)

Page I of 1

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a Setailed Quallfications aEld Froficlemcy Test Report*ate; 212812007

?eport ilescription:\TU Personnel use this

Toxicology

QualifioUons Date

LlIlL999 12:00:00AM

to view detalled ifications and

Quantibtive - Drug Analysis


L2lL6lt999 12;00;00AM

Expiration Date without a new PT

512512002 1l:59:SBPM


QuaftypeLinklD

000000000000275

Detailed Qualifications and Froficiency Tast Repont for MADELINE A MONTGOMER.Y 07It-0S00


Identifier 99-18A

Staff Position CHEMIST-FORENSIC EGMINERTest Source External


Supplier CAP

Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification of Test 5/1/2000 12:00:00AMLD-PTPM Review Notlfled


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

LllLl1999 12:00:00AM

LZlt6lL999 12:00:00AM

tZlL0lL999 12:00:00AM

51212000 12:00:00AM

.ntifier 00-17

,ff Position CHEMIST-FORENSIC EGMINER


Source Unit


Preparer Name

Verifier Name

Validator Name

LT-PTPM Noufication of TeSt 5/7 12001 12:00:00AMLD-PTPM Review NoUfied


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

ILl612000 12:00:00AM

t2/21/2000 11:59:59PM

1212612000 12:00:00AM

5l14/2001 12:00:00AM

Identifier 01-3

stAff Position CHEMIST.FORENSIC EKAMINER



Supplier CAP

Preparer Name

Verifier Name

Validator Name




LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

3lL6l200L 12:00:00AM

412612001 12;00:00AM

41201200L 12:00:00AM

614/200t 12:00:00AM

6/5/2041 12:00:00AM

6151200t 12:00:00AM

61412001 12:00:00AM

Identifier 02-4

Staff Position CHEMIST-FORENSIC E0MINERTest Source External

'rce Unit


Preparer Name

Verifier Name

Validator Name

5) qqcvtner comments

(,o's

Setal$ed atificatlems arnd Fnoff,cfencv T'est R

*are; 2l2Bl20Q7

-eport Fescripticn:

[!_fg1so-nnel use this report to view detailed qualifications and test for selected staff.

Distribution Date 312S1ZOOZ !Z:OO:ODue Date 5?4l2ooz 11:59:59pM LD-prpM Review NoufiedPT Complete Date SI2IZOOZ 12:00:00AM UC Designee Final EvalTestee Feedback LL14/ZOOI 12:00:O0AM LD-pTpM Eval

Detailed Qualifications and Froficiency Test Report for MADELINE A Mor.{TGOMERY 0731-0000

{* +v^( t: rZ)na^^ .?

^3 -t

Setailed &saFlficatios'rs and frsfici Test Repoft*ate: 212812007

'eport Description:rTU Personnel use this to view detailed test for selected staff.

Toxicology

Qualifications Date

7/t12002 12:00:00AM

Quantitative - Drug Analysis

Most Recent Proficienry Test

511412003 11:59:59PM

Expiration Date without a new PT

L211712007 11:59:58PM

QualTypeLinkID

000000000000276

Oetailed Qualifications and Proficiency Test Report for IvIADELINE A MONTGOMERY 0791-0000

Identlfier 02-12A

Staff Position CHEMIST-FORENSIC EXAMINER


Source Unit

Supplier College of American PathologisbPreDarer Name

Verifier Name

Validator Name

LT-mM NoUflcation of Test 8/16/2002 12:00:00AMLD-FTPM Review Notified


LD.PTPM EVaI

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

7/2/2002 12:00:00AM

7lt5l2002 11:59:59PM

7/9/2002 12:00:00AM

ItlL5l2002 12:00:00AM

'ntifier 03-4A

-.aff Position CHEMIST-FORENSIC EXAMINER

Test Source Extemal

Source Unit


Preparer Name

Verifier Name

Validator Name

LT-mM NotificaUon of fegr 4/ZS1Z003 12:00:00AMLD-PTPM Review Notified


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

312612003 12;00:00AM

511412003 11:59:59PM

4/25/2003 12:00:00AM

712912003 12:00:00AM

Identifier 04-20A

StAff Position CHEMIST.FORENSIC ENMINERTest Source External

Source Unit


Preparer Name

Verifier Name

Validator Name

LT-my Notificauon of Test 1/18/2005 12:00:00AMLD-PTPM Review Notified


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

L0/2612004 12:00:00AM

1211612004 12:00:00AM

LL/9/2004 12:00:00AM

Identifier 05-238

Staff Position


rrce Unit

other Comments


Preparer Name

Verifier Name

Validator Name

UY VVb/\(bao1

Setnlled uallfications amd Fs'oficierucy ?est Reaate: 212812007

oeport Description:rTU Personnel use this to view detailed qualifications and test for selected staff.

Oetailed Qualifications and Proficiency Test Report for MADE!-trNE A MONTGOMERY 073t.-0S00

Due Date

PT Complete Date

Testee Feedback

Ltl712005 12:00:00AM

t21L612005 11:59:59PM

L211412005 12:00:00AM

121t412006 12:00:00AM

LT-PTPM



LD-PTPM Eval

t21L412005 12:00:00AM

Identifier 06-34

Staff Position

Test Source E*ernal

Source Unit

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

312212046 12:00:00AM

5/812006 11:59:59PM

411312006 12:00:00AM

16i2006 12:00:00AM


Preoarer Name

Verifier Name

Validator Name

LT-PTPM NoUfi cauon of T etr 4 I L3 12006 12:00:00AMLD-FIPM Review NoUfied


LD-PTPM Eval

E, q4'1o'4Faqe 2 of 2

. ;:{

Detailed arailficatlsns and Fnsfic[e*ate: 2128120Q7

Report Description:\TU Personnel use this to view detailed ifications and test for selected staff.

Toxicology

Qualifications Date

71t12002 12:00:00AM

Qualitative - Drug Analysis


5/14/2003 11:59:59PM



L211512007 11:59:58PM 000000000000274

Detailed Qualifications and Froficiency Test Report for MADELINE A MONTGOMERY 0Ig1-0000

ryryWW q I I I { { i I dws.'I {:1 a KTJTFI n ff*l ff-;K I I I J I I | | yJ : ts WgreffiWre

IdenUfier 02-12A

StafF Position CHEMIST-FORENSIC EXAMINER


Source Unit

Supplier College of American Pafrologists

Preparer Name

Verifier Name

Validator Name

LT-PTPM Notifi cation of Test 8/16/2002 12: 00:00AMLD-PTPM Review NoUfied


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

712/2002 12:00:00AM

711512002 11:59:59PM

7/9/2007 12:00:00AM

Ltlt5l2002 12:00:00AM

312612003 12:00:00AM

51L412003 11:59:59PM

4/2512003 12:00:00AM

712912003 12:00:00AM

rnUfier 03-4A

.rff Position CHEMIST-FORENSIC EXAMINER


Source Unit


Preparer Name

Verifier Name

Validator Name

LT-ffiM Notifi cation ot Test 4 l2S/2003 12:00:00AMLD-PFPM Review Notified


LD-PTPM EVaI

Identifier 04-204

Staff Position CHEMIST-FORENSIC EKAMINER


Source Unit


Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification of Test 1/19/2005 12:00:00AMLD-PTPM Review NoUfied


LD-PTPM Eval


Preparer Name

Verifier Name

Validator Name

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

Identifier 05-238

Staff Position


'rrce Unit

wcher Comments

1012612004 12:00:00AM

L2/t612004 12:00:00AM

LUgl2A04 12:00:00AM

Ll1812005 12:00:00AM

+ 4&-b2^

ffietaiBed uaE$ficatiosls arnd FnoSIci

*ate: 212812007

aeport Description:\TU Personnel use this to view detailed oualifications and test for selected staff.

Detailed Qualifications and Profrciency Test Repo* for MADELINE A MONTCOMERY 0731-00$$

LIl712005 12:00:00AM

LZlL4l2005 11:59:59PM

L211412005 12:00:00AM

L211412006 12:00:00AM

LT-FIPM NotiflcaUon of Test L21L412005 12:00:00AMDue Date

PT Complete Date

Testee Feedback



LD-PTPM Eval

Identifier 06-3A

Staff Position

Test Source E*ernal

Source Unit

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

Supplier

Preparer Name

Verifier Name

Validator Name

College of American Pathologists

312212006 12:00:00AM

51812006 11:59:59PM

41t312006 12:00:00AM

LT-PTPM NoUfication of Test

LD-P|PM Review Notifled


LD.PTPM EVaI

41t312006 12:00:00AM

16/2006 12:00:00AM

5o qVa( c' az)

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SetaiHed Qua6liicatiorss arrd Proficfiency Test Repo$sat* 212812007

-eport Sescniption:,TU Personnel use this to view detailed ualifications and

Toxicology

Qualifications Date

tltlL999 12:00:00AM

QualitaUve - Drug Analysis


512412002 11:59:59PM


Sample Prep,,Wet Chem. & Inst. Analysis

Expiration Date without a new pT eualTypeLinklD

5/25/2002 11:59:58PM 000000000000273

Detailed Qualifications and Proficiency Test Report for M^ADEUNE A MoNTGoMERy 0731-0000

Identifier 994Staff Position CHEMIST-FORENSIC E0MINERTest Source Extemal


Supplier CAP

Preparer Name

Verifier Name

Validator Name




LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

3lL7/1999 12:00:00AM

312911999 12:00:00AM

7121t999 12:00:00AM

8141t999 12:00:00AM

3lL7/1999 12:00:00AM

7lI3lL999 12:00:00AM

8/10/1999 12:00:00AM31t512000 12:00:00AM

ntifier 00-6

-,aff Position CHEMIST-FORENSIC E0MINERTest Source External


Supplier CAP

Preparer Name

Verifier Name

Validator Name

LT-FIPM NoUfication of Test

LD-ffPM Review Notified


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

61712000 12:00:00AM

6/t912000 12:00:00AM

611912000 12:00:00AM

8/30/2000 12:00:00AM

8/30/2000 12:00:00AM

8/30/2000 12:00:00AM

812912000 12:00:00AM

Identifier 01-3


Test Source Extemal


Supplier CAP

Preparer Name

Verifler Name

Validator Name

LT-PTPM NoUfi cation of Test

LD-ffPM Review Noufied


LD-PTPM Eval

Other Comments

Distrlbution Date

Due Date

ff Complete Date

Testee Feedback

3/16/200t 12:00:00AM

312912001 12:00:00AM

3/281200t 12:00:00AM

6/4/200t 12:00:00AM

6/5/2001 12:00:00AM

6/51200L 12:00:00AM

61412001 12:00:00AM

Identifier 02-4

Staff Position CHEMIST-FORENSIC EKAMINER


rrce Unit


Preparer Name

Verifier Name

Validator Name

Ew,Other Comments

b2c

*sta!$ed QLsa$ffficatfiorns amd Fnoficiency Test*at€: 2/2812007

-epoft Eescription;rTU Personne_!,use this report to view detailed test for selected staff.

Detailed Qualifications and Proficiency Test Report for MADELINE A MoNTGoMERy 0731-0000

DistribuUon Date 3/25/200t 12Due Date 5/2412002 l1:59:59pM LD-pTpM Review NotifiedPT complete Date sl2l20o2 12:00:00AM uc Designee Final EvalTestee Feedback Ltl4lZO}Z 12:00:00AM LD_pTpM Eval

[, qu^(o as)

Fage 2 of 2

Date: 212812007

-epott Description:ATU Personnel use this to view detailed

N1o-fEciency Test Repoft


Toxicology

QualificaUons Date

7/L/2002 12:00:00AM

Blood Alcohol


7/712003 11:59:59PM


Expiration Date without a new pT Qual[ypeLinklD

LZl2l2007 11:59:58PM 000000000000272

Detailed Qua$ifications and

Detailed Qualifications and Proficiency Test Report for MADELINE A MoNTGoMERy 0731-0000

Identifier 02-12A



Source ljnit

Other CommenE

Distribution Date TZ|ZOOZ 12:00:00AMDue Date 7ftSlZOO2 11:59:59pMPT Complete Date TpnOOZ t2:00:00AMTestee Feedback

Supplier College of American pathologisE

Preparer Name

Verlfier Name

Validator Name

LT-PTPM NoUfi cation of 'f e*. 7 / tS 12002 12:00:00pMLD-PTPM Review Notifled


LD-PTPM Eval

ntifier 03-9A

-Laff PosiUon CHEMIST-FORENSIC EXAMINER


Source Llnit


Preparer Name

Verifier Name

Validator Name

LT-PTPM Notifi cation of TesI 7 / Ll 2003 12:00:00AMLD-FIPM Review NoUfied


LD-PTPM Eval

Other Ccmmen6

Distribution Date

Due Date

PT Complete Date

Testee Feedback

6/23/2003 12:00:00AM

71712003 11;59:59PM

7/t12003 12:00:00AM

712912003 12:00:00AM

Identifler 04-2A



Source Unit

Other Comments

Distribution Date 3D12OO4 12:00:00AMDue Date 3123/2004 11:59:59pMPT Complete Date 3fl7lZOO4 12:00:00AMTestee Feedback 4lL2l2OO4 12:00:00AM


Preoarer Name

Verifier Name

Validator Name

LT-P|PM Notification of Test 3/1712004 12:00:00AMLD-PTPM Review NoUfied


LD-PTPM Eval

Identifier 05-3A supplier college of American pathologisEStaff Position preparer NameTest Source External Verifier Name

'rce Unit Validator Name

Other Cornments CAP #&5L70LlALI-A: satisfactory completion

t/(b( oac

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Setailed Qe,ua$$ficat!CIms and FnofE

Datet 212812007

eepod Description:tTU Personnel use this to view detailed oualifications and test for selected staff.

Detailed Qualifications and Proficiency Test R.eport for MADELINE A MONTGOMER.Y 0731-0000

Distribution Date 31812005 12:00:00AM LT-PTPM Notification of Test 3/11i2005 12:00:00AM

Due Date 3lZZlZ00S 1t:59:59pM LD-PTPM Review Notified

PT Complete Date 3lfil1111 1Z:00:00AM UC Designee Final Eval

Testee Feedback 7ltBlZ}lS 12:00:00AM LD-PTPM Eval

Identifler 06-22A Supplier Collaborative Testing Services

Staff Position Preparer Name

Test Source External Verifier Name

Source Unit Validator Name

Other Comments

Distribution Date to/10/2006 12:00:00AM LT-PTPM Notification ofTest 11/20/2006 12:00:00AM

Due Date rzlLlzoo6 11:59:59pM LD-PTPM Review Notified

PT Complete Date Lllzol2oo6 t2:00:00AM UC Designee Final Eval

Testee Feedback ZlLl2007 12:00:00AM LD-PIPM Eval

6 +vu(uat)

Faqe 2 af 2

Setal$ed SuaEiliicatioms amd Froflcie Test Re

Date: 212812007

4.epott Descripticn:\TU Personnel use this to view detailed ions and test for selected staff.

Toxicology

Qualifications Date

Lll/L999 12:00:00AM

Blood Alcohol


Sample Prep,,Wet Ctem. & Inst. Analysis

ExpiraUon Date without a new PT Qual-l-ypeUnklD

000000000000225

Identifier 99-7




Supplier CAP

Preparer Name

Verifier Name

Validator Name

LT-FfPM Notification of Test 6/15/1999 12:00:00AMLD-PTPM Review Notified 612411999 t2:00:00AMUC Designee Final Eval 8/10/1999 12:00:00AMLD-PTPM Eval 3lt5l2000 12:00:00AM

Supplier CAP

Preparer Name

Verifier Name

Validator Name

LT-PTPM Notificauon 0f Test 12118/2000 12:00:00AM

LD-PTPM Review Noufied tzltBlZ000 12:00:00AM

UC Desisnee Final Eval 121412000 12:00:00AMLD-PTPM Eval

,ntifier 00-12

:ff Position CHEMIST-FORENSIC EXAMINER

Test Source Extemal


Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

6lt5l|999 12:00:00AM

61251t999 12:00:00AM

61221t999 12;00:00AM

8141t999 12:00:00AM

9/1912000 12:00:00AM

9l2912OOO 12:00:00AM

9/2912000 12:00;00AM

L211812000 12:00:00AM

Identifier 01-68




Supplier CAP

Preparer Name

Verifier Name

Validator Name

LT-PTPM Notiflcation of Test.. 71212001 12:00:00AMLD-PTPM Review Notified 7/2la00t 12:00:00AMUC Designee FinalEval 71212001 12:00:00AMLD-PTPM Eval

5lt4lz00tsl23l200rsl2Ll200L

12:00:00AM

12:00:00AM

12:00:00AM

12:00:00AM

{* uot( tr t*)

Faae L of 1

CIetailed Qualification$ and Proficiency Test Report for MADELINE A MONTGOMER.Y 0731-0S00

Bwffi#ffie$ffi q r il-a {ii i$fr;\ a;l i g cll}-l n iT-il {Ffig r i r I r l il | r# !.: ;ffi8n

7 t2t2001

FetaEled uaBlficatloils and Froflciency Test Report*at*; 212812007

qepogt sescription;tTU Personnel use this to view detailed ifications and test for selected staff.


Qualifications Date

7/t12002 12:00:00AM

Drug Analysis


911012003 11;59:59PM


Expiration Date without a new PT QuatTypeLinklD

912312007 l1:59:58PM 000000000000224

Oetailed Qualifications and Frcficiency Test Report for MADELINE A MOr-|TGOMERY 0731-0000

Identifier 03-12A



Source Unit


Preparer Name

Verifier Name

Validator Name

LT-PTPM Noufication of Test 8/13/2003 t2:00:00AMLD-PTPM Review NoUfied


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

7/30/2003 12:00:00AM

911012003 11:59:59PM

B/13/2003 12:00:00AM

L2/212003 12:00:00AM

'ntifier 04-13A

.rff Position CHEMIST-FORENSIC EXAMINER


Source Unit


Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification of Test 10/2612004 12:00r00AMLD-PTPM Review Notifled


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

7/L512004 12:00:00AM

Bl26l20M 11:59:59PM

L0/2612004 12:00:00AM

1012612004 12:00:00AM

Identifier 05-15A

Staff Position

Test Source Extemal

Source Unit

Other Comments CTS 05-502- saUsfactory completion

Distribution Date BIfiIZOOS 12:00:00AMDue Date 9lZ3lZ00S 11:59:59pMPT Complete Date yL2lz005 12:00:00AMTestee Feedback L1.lLlZ}lS 12:00:00AM

Supplier CollaboraUve Testing Services

Preparer Name

Verifier Name

Validator Name

LT-PTPM Notification of lesI 91L212005 12:00:00AMLD-P|PM Review Notified


LD-PTPM Eval

Identifier 06-3A

Staff Position


rrce Unit

uther Comments Mistaken entry


Preparer Name

Verifier Name

Validator Name

[r ,tqb( aa'lagelt3

setaiHed Q{ea$fficat$orss and Fnof$ciemcy Test ReportDate: 2/2812007

qeport Description:rTU Personnel use this to view detailed qualifications and test for selected staff.

Detailed Qualifications and Froficiency Test Report for MADELINE A MoNTsoMER.y 0731-0000

Distribution Date

Due Date

PT Complete Date

Testee Feedback

3/2212006 12:00:00AM

51812006 11:59:59PM

Notification of T

LD-ffiM Review Notified


LD-PTPM Eval

Identifier 06-174

Staff Position

Test Source Extemal

Source Unit

Other CommenE

Distribution Date

Due Date

PT Complete Date

Testee Feedback

8/10/2006 12;00:00AM

912212005 11:59:59PM

91t412006 12:00:00AM

12/412006 12:00:00AM


Preparer Name

Verifier Name

Validator Name

.LT-PTPM Noufication of TesI 91t412006 12:00:00AMLD-ffiM Review NoUfied


LD-F:I-PM Eval

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*eta!led QualEflcations and FroficleDatet, 212817007

aeport Description:\TU Personnel use this to view detailed fications and test for selected staff.

Detailed Qualifications and Froficiency Test Report for MADEUNE A MONTGOMERY 0731-0000

W6&Wggffi qrmTff &'t EI i 4rtrFl n rrfr I ir'IEn I I I I t I I I I tJ : g ffi f EFWil


QualificaUons Date

IlLlL999 12:00:00AM

Drug Analysis



Expiration Date wlthout a new PT QualTypeLinklD

000000000000223

Identifier 99-148

Staff Position CHEMIST-FORENSIC EUMINER



Supplier CIS

Preparer Name

Verifier Name

Validator Name

LT-ffPM NoUfi cation of Test



LD-PTPM Eval

Other Comments

DistribuUon Date

Due Date

PT Complete Date

Testee Feedback

L0ltl1999 12:00:00AM

tLlL9lt999 12:00:00AM

LLl4lL999 12:00r00AM

212912000 12:00:00AM

212912000 12:00:00AM

2l29l2OOO 12:00:00AM

212812000 12:00:00AM3/15/2000 12:00:00AM

rntifier 00- 11C

-dff Position CHEMIST-FORENSIC EOMINER


Source Unit ChemisW Unit

Supplier CTS

Preparer Name

Verifier Name

Validator Name

LT-P|PM Noufication of Test



LD-PTPM EVaI

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

813112000

10/30/20oo

10/16/2000

L?/L8t2000

12:00:00AM

12:00:00AM

12:00:00AM

12;00:00AM

L2lLBl2000 12:00:00AM

L211812000 12:00:00AM

1211812000 12:00:00AM

fo u+1-( r"l,;

Page 1 of 1

\

sate: 2/2812007

sl.epott Descniption;ATU Personnel use this to view detailed ifications and test for selected stafi.

Setalled ua$*fications amd Froflciency Test Report


Qualifications Date

L/t/1999 12:00:00AM

Drug Analysis


Iol8l2o04 12:00:0bAM


ExpiraUon Date without a new PT QualTypeLinKD

912312007 11:59:58PM 000000000000224

Detailed Qualifications and Proficiency Test Report for EILEEN MARIE WANINGER 0731-00S0

Identifier 99-5E




Supplier CTS

Preparer Name

Verifier Name

Validator Name




LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

5l18/1999 12:00:00AM

7lB/L999 12:00:00AM

61291t999 12:00:00AM

81411999 12:00:00AM

7ll3lt999 12:00:00AM

7/131t999 12:00:00AM

8/10/1999 12:00:00AM31t512000 12:00:00AM

ntifier 00-3D

-aff Position CHEMIST-FORENSIC ryAMINER

Test Source E*ernalSource Unit Chemistry Unit

Supplier CfsPreparer Name

Verifier Name

Validator Name

LT-F|PM NoUfication of Test

LD-PfPM Review NoUfied


LD-PTPM Eval

Other Commenb

Distribution Date

Due Date

PT Complete Date

Testee Feedback

51312000 12:00:00AM

6/2812000 12:00:00AM

612012000 12:00:00AM

8/7/2000 12:00:00AM

8/7/2000 12:00:00AM

8/712000 12:00:00AM

712812000 12:00:00AM

Identifier 01-5A

Staff Position CHEMIST-FORENSIC E0MINERTest Source External


Supplier CTS

Preparer Name

Verifier Name

Validator Name

LT-PTPM NoUfication of Test



LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

3/2I/2001 12:00:00AM

5/17/200L 12:00:00AM

4lt0l200L 12:00:00AM

6/Lt/200L 12:00:00AM

6lL2l200t 12:00:00AM

6lL2l200L 12:00:00AM

611112001 12:00:00AM

Identifier 02-lCStaff Position CHEMIST-FORENSIC EGMINER


'ce Unit


Preparer Name

Verifier Name

Validator Name

V((,bu)

&uther Comments

Detailed Qssalificatloffis and Fnoflciemcy Test R.epoft

Sate: 2/2812007

Deport Description;rTU Personnel use this

Distribution Date

Due Date

PT Complete Date

Testee Feedback

31812002 12:00:00AM

412617002 11:59:59PM

31t512002 12:00:00AM

71112002 12:00:00AM

rt to view detailed ualifications and

LT-PTPM Notification esl T | 112002 12:00:00AM



LD-PTPM Eval


Setailed Qualifications and Proficiency Test Report for EILEEN MARIE WANINGER 0731-00S0

Identifier 03-1D



Source Unit

Other CommenE

Distribution Date

Due Date

PT Complete Date

Testee Feedback


Preparer Name

Verifier Name

Validator Name

LT-PTPM Notiflcation of Test 41L512003 12;00:00AM


UC Designee Flnal Eval

LD-PTPM Eval

3lL7lZ003 12:00:00AM

412912003 11:59:59PM

411512003 12:00:00AM

91312003 12:00:00AM

Identifier RE031007012

Staff iosition CHEMIST-FORENSIC EXAMINER


Source Unit

rer Comments LD-QAM required re-examination for 2003.

Distribution Date 1U19/2003 12:00:00AM

Due Date t213112003 11:59:59PM

PT Complete Date 121212003 12:00:00AM

Testee Feedback

Supplier Re-Examination

Preparer Name

Verifier Name

Validator Name

Controlled Substances




LD-PTPM Eval

Identifier 04-13D

Staff PositioN CHEMIST.FORENSIC EXAMINER


Source Unit


Preparer Name

Verifier Name

Validator Name

LT-PTPM Noufication of Test 10/2612004 12:00:00AM



LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

7/t512004 12:00:00AM

817612004 11:59:59PM

712712004 12:00:00AM

t012612004 12;00:00AM

Identifier 05'15D

Staff Position


Source Unit

Other Comments

Distribution Date

^'re Date

Complete Date

r estee Feedback

CTS 05-502-saUsfactory completion

B/10/2005 12:00:00AM

912212005 11:59:59PM

8/2412005 12:00:00AM

1U1l2005 12:00:00AM


Preparer Name

Verifier Name

Validator Name

LT-ffPM Notification of TesI 812412005 12:00:00AM

LD-P-[PM Review Notified


LD-PTPM Eval

f* vq( uzt

SstaiBed Suse$lflcatiosls amd Fnoficie Yest Repoffisate: 2/2812007

-epo* Description:ATU Personnel use this to view detailed test for selected staff.

Detailed Qualifications and Prcflciency Test R.epcrt for EILEEN MAruE WAHINSER 0731-0000

Identifier 06-17C Supplier CollaboraUve Testing Services

Staff Position Preparer Name

Test Source External Verifier Name

Source Unit Validator Name

Other Comments

Distribution Date 8ln?006 12:00:00AM LT-PTPM Noufication of Test 8/10/2006 12:00:00AM

Due Date 912212006 11:59:59PM LD-FrPM Review Noufled

rr complete Date 91712006 12:00:00AM UC Designee Final Eval

Testee Feedback 121412006 12:00:00AM LD-PTPM Eval

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ffietaiEed q.sallfications amd Freficle Test R

Dat"et 212812007

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Setailed Qualifications and Proficiency Test Report for EILEEI{ MARIE WANINGER 0731-00S0

WWffW4Tr-{TnW-'{f; liqelrFlnrrfr i{T:rIGKrlrlf lll{tliF&mffi W&ffi @F

Trace Analysis (Chem.)

Qualifications Date

LlLlL999 12:00:00AM

Bank Dyes


L012312003 11:59:59PM


Expiration Date without a new PT Quafl'ypeLinklD

812L12007 11;59:59PM 000000000000261

Identifier 99-3F




Supplier

Preparer Name Wang, Deborah

Verifier Name

Validator Name

LT-FrPM Noufication of :]5I 5lL7lL999 12:00:00AM

LD-PTPM Review Notified SlL7lL999 12:00:00AM

UC Designee Final Eval 51411999 12:00:00AMLD-PTPM Eval 3/1s/2000 12:00:00AM

Supplier

Preparer Name Cook, Pamela C.

Verifier Name

Validator Name

Ofier Commenb Test 00-B was withdrawn and a new test was reissued.




LD-PTPM Eval

Supplier

Preparer Name Cook, Pamela C.

Verifier Name

Validator Name

LT-FrPM Notification of Test 12118/2000 r2:00:00AMLD-PTPM Review NoUfled !2/1812000 12:00:00AM

UC Desisnee FinalEval 1211812000 12:00:00AMLD-PTPM Eval

Supplier

Preparer Name Wang, Deborah

Verifier Name

Validator Name

fo uvt

rtifier 00-8C

-.aff Position CHEMIST-FORENSIC E$MINER

Test Source internal


bther Comments

DistribuUon Date

Due Date

PT Complete Date

Testee Feedback

Distribution Date

Due Date

PT Complete Date

Testee Feedback

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

3/t61L999 12:00:00AM

41271t999 12:00:00AM

3/261L999 12:00:00AM

41271L999 l2:00:00AM

711012000 12:00:00AM

Bl2Il2O00 12:00:00AM

9/2612000 12:00:00AM

Ltl9l2000 12:00:00AM

912812000 12:00:00AM

LZlt9l2000 12:00:00AM

Identifier 00-14D

Staff Position CHEMIST-FORENSIC E$MINER



Identifier 01-11C

Staff Position CHEN4IST-FORENSIC EXAMINER

Test Source Intemal

rce Unit Chemistry Unit

Other Comments

b3s

Setai[ed X$ficatias, s and Pogftgtency Test Report&ate: Zl2el2007

ceport Description:rTU Personnel use this

bution Date

Due Date

PT Complete Date

Testee Feedback

to view detailed

71L912001. 12:00:00AM

8/3012007 12:00:00AM

7/3112001 12:00:00AM

91251200t 12;00:00AM



LD-PTPM Eval

test for selected staff,

912512001 12:00:00AM

91251200t 12:00:00AM

912512001 12:00:00AM

Detailed Qualificaticns and Proficiency Test Report for EILEEN MARIE WANINGER 0731-0000

Identifier 02-168

Staff Position CHEMIST-FORENSIC EGMINERTest Source Intemal

Source Unit D7-LABORATORY DIVISION

Supplier

Preparer Name DEBOMH WANG

Verifier Name MICHAEL P RICKENBACH

Validator Name DEBOMH WANG

LT-PrPM Noufication ofTest 10/2512002 9:00:00AMLD-ffPM Review NoUfied


LD-PTPM Eval

Other Comments

DistribuUon Date

Due Date

PT Complete Date

Iestee Feedback

9/2612002 5:00:00PM

ttl8l2002 12:00:00AM

L0/24/2002 12:00;00PM

t2l9/2002 12:00:00AM

Identifler 03-13C

Staff Position CHEMIST-FORENSIC EGMINERTest Source Internal

SourceUnit D7-CHEMISTRY

Supplier


Verifier Name MICHAEL p RICKENBACH


LT-PTPM NotlficaUon of Test 10/3/2003 12:00:00AMLD-PTPM Review NoUfied


LD-PTPM Eval

er Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

9lLLl2003 12:00:00AM

LO/2312003 11:59:59PM

101312003 12:00:00AM

L0/2712003 12:00:00AM

Identifter 04-BC

Staff Position CHEMIST-FORENSIC EOMINER

Test Source Intemal

Source Unit CU

Supplier


Verifier Name ROBERT F MOTHERSHEAD


LT-PTPM Notjfication of TesI 6n012004 12:00:00AMLD-PTPM Review Notified


LD-PTPM Eval

Other Comments

Distribution Date

Due Date

PT Complete Date

Testee Feedback

6/23/2004 12:00:00AM

8/412004 11:59:59PM

613012004 12:00:00AM

6/30/2004 12:00:00AM

Identifier 05-10C

Staff Position


Source Unit CHEMISTRY

Other Comments

Distribution Daten're Date

:omplete Date

r estee Feedback

TEST SET #1- satisfactory compleuon

5/18/2005 12:00:00AM

6129/2005 11:59;59PM

5/1812005 12:00:00AM

8lLLl2005 12:00:00AM

Supplier


VerifierName ROBERTMOTHERSHEAD

Validator Name DEBORAH WANG

LT-PTPM Noufication of Test 5/19/2005 12:00:00AMLD-PTPM Review Notified


LD-PTPM Eval

&,/,1,b)t

Setalled Qura$$ficatiosls and Froficiency Test Reportsate: 2/2812007

oeport Sescription:.\TU Personnel use this to view detailed test for selected staff.

Detailed Qualifications and Proficiency Test Report for EILEEN MARIE WANINGER 0731-0000

Identifier 06-258 Supplier

Staff Position Preparer Name Pamela Reynolds

Test Source Internal Verifier Name Eileen Waninger

Source Unit Chemistry Validator Name Jason Brewer

Other Comments

Distribution Date 5/18/2006 12:00:00AM LT-PTPM Nouflcation ofTest 5/2612006 12:00:00AMDue Date 613012006 11:59:59PM LD-PTPM Review Noufied

PT Compfete Date 512612006 12:00100AM UC Designee Final Eval

Testee Feedback 6lL'lz006 12:00:00AM LD-FTPM Eval

4(6(aslPase 3 of3

trial exhibit 446

Documents