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  • MT-605

    Riboflavin, [3H]-

    Lot 213-021-0212-A-20090119-JG

    A) All chromatograms were run using the HPLC method described on the Product Data Sheet.

    Concentrations and volumes:

    Standard solution concentration was 0.5 mg/ml.

    Riboflavin, [3H]- concentration was 0.2 mCi/ml. Volume of standard alone injection was 2.0 µl.

    Volume of Riboflavin, [3H]- alone injection was 1.0 µl.

    Co-injection solution consisted of 1.5 µl Riboflavin, [3H]- + 2.0 µl standard.

    Volume of co-injection was 3.5 µl.

    Volume of blank injection was 1.0 µl.

    B) Mass spectrometry – Positive mode C) NMR

  • MT-605Riboflavin, [3H]-

    Lot 213-021-0212-A-20090119-JG

    Chromatogram Info:

    File Name : L:\int21138 File Created : 2/25/2014 10:51:06 AM

    Origin : Acquired, Acquisition started 5/17/2011 3:05:10 PM Acquired Date : 5/17/2011 3:25:10 PM

    Project : Test By : Administrator

    Method : unit2-20minrun By : Administrator

    Description : Radiochemical trace of 3H material alone

    Created : 8/8/2007 9:12 AM Modified : 2/25/2014 11:03 AM

    Column : Detection : Radiochemical

    Mobile Phase : Temperature :

    Flow Rate : Pressure :

    Note :

    [min.]Time

    5 10 15 20

    [mV]

    Volta

    ge

    0

    100

    200

    300

    400

    500

    3.62

    1

    4.26

    2

    4.73

    3

    5.42

    4

    7.92

    5 L:\ int 21138 - Unit 2 Radio

    2/25/2014 11:04 AM Page 1 of 2Chromatogram L:\int21138.PRM

  • Result Table (Uncal - L:\int21138 - Unit 2 Radio)

    CompoundName

    Reten. Time[min]

    Area[mV.s]

    Height[mV]

    Area[%]

    Height[%]

    Efficiency[th.pl]

    Eff/l[t.p./m]

    Symmetry/Tailing[-]

    Response Factor

    Resolution[-]

    1 3.62 39.296 2.49 0.31 0.53 995.86 19917.25 1.15

    2 4.26 69.916 4.31 0.55 0.92 1900.52 38010.47 0.78 1.5

    3 4.73 168.914 8.24 1.33 1.77 2343.02 46860.44 1.52 1.2

    4 5.42 35.916 1.48 0.28 0.32 1188.79 23775.79 3.08 1.4

    5 7.92 12364.257 449.73 97.52 96.46 2406.54 48130.78 1.55 3.9

    Total 12678.298 466.24 100.00 100.00

    2/25/2014 11:04 AM Page 2 of 2Chromatogram L:\int21138.PRM

  • MT-605Riboflavin, [3H]-

    Lot 213-021-0212-A-20090119-JG

    Chromatogram Info:

    File Name : L:\int21138 File Created : 2/25/2014 10:51:06 AM

    Origin : Acquired, Acquisition started 5/17/2011 3:05:10 PM Acquired Date : 5/17/2011 3:25:10 PM

    Project : Test By : Administrator

    Method : unit2-20minrun By : Administrator

    Description : UV trace of 3H material alone

    Created : 8/8/2007 9:12 AM Modified : 2/25/2014 11:02 AM

    Column : Detection : UV 266nm

    Mobile Phase : Temperature :

    Flow Rate : Pressure :

    Note :

    [min.]Time

    5 10 15 20

    [mV]

    Volta

    ge

    -2

    0

    2

    4

    6

    8

    7.72

    1

    L:\ int 21138 - Unit 2 UV

    2/25/2014 11:02 AM Page 1 of 2Chromatogram L:\int21138.PRM

  • Result Table (Uncal - L:\int21138 - Unit 2 UV)

    CompoundName

    Reten. Time[min]

    Area[mV.s]

    Height[mV]

    Area[%]

    Height[%]

    Efficiency[th.pl]

    Eff/l[t.p./m]

    Symmetry/Tailing[-]

    Response Factor

    Resolution[-]

    1 7.72 26.518 1.98 100.00 100.00 8833.46 176669.22 0.87

    Total 26.518 1.98 100.00 100.00

    2/25/2014 11:02 AM Page 2 of 2Chromatogram L:\int21138.PRM

  • MT-605Riboflavin, [3H]-

    Lot 213-021-0212-A-20090119-JG

    Chromatogram Info:

    File Name : L:\int21139 File Created : 2/25/2014 10:51:06 AM

    Origin : Acquired, Acquisition started 5/17/2011 3:44:42 PM Acquired Date : 5/17/2011 4:04:42 PM

    Project : Test By : Administrator

    Method : unit2-20minrun By : Administrator

    Description : UV trace of standard material alone

    Created : 8/8/2007 9:12 AM Modified : 2/25/2014 11:05 AM

    Column : Detection : UV 266nm

    Mobile Phase : Temperature :

    Flow Rate : Pressure :

    Note :

    [min.]Time

    5 10 15 20

    [mV]

    Volta

    ge

    0

    100

    200

    300

    400

    4.50

    1

    5.22

    2

    7.70

    3

    8.44

    4

    9.32

    5

    9.82

    6

    L:\ int 21139 - Unit 2 UV

    2/25/2014 11:05 AM Page 1 of 2Chromatogram L:\int21139.PRM

  • Result Table (Uncal - L:\int21139 - Unit 2 UV)

    CompoundName

    Reten. Time[min]

    Area[mV.s]

    Height[mV]

    Area[%]

    Height[%]

    Efficiency[th.pl]

    Eff/l[t.p./m]

    Symmetry/Tailing[-]

    Response Factor

    Resolution[-]

    1 4.50 19.845 2.42 0.42 0.66 7779.09 155581.75 0.82

    2 5.22 18.157 1.23 0.39 0.34 7711.68 154233.66 1.03 3.3

    3 7.70 4623.817 359.77 98.90 98.71 9418.50 188369.93 1.34 8.9

    4 8.44 4.427 0.36 0.09 0.10 9865.85 197317.07 1.16 2.3

    5 9.32 3.780 0.30 0.08 0.08 11639.23 232784.70 0.99 2.6

    6 9.82 5.050 0.40 0.11 0.11 12516.61 250332.16 1.01 1.4

    Total 4675.075 364.48 100.00 100.00

    2/25/2014 11:05 AM Page 2 of 2Chromatogram L:\int21139.PRM

  • MT-605Riboflavin, [3H]-

    Lot 213-021-0212-A-20090119-JG

    Chromatogram Info:

    File Name : L:\int21140 File Created : 2/25/2014 10:51:06 AM

    Origin : Acquired, Acquisition started 5/18/2011 8:52:45 AM Acquired Date : 5/18/2011 9:12:45 AM

    Project : Test By : Administrator

    Method : unit2-20minrun By : Administrator

    Description : Radiochemical trace of 3H material co-injected with standard

    Created : 8/8/2007 9:12 AM Modified : 2/25/2014 11:06 AM

    Column : Detection : Radiochemical

    Mobile Phase : Temperature :

    Flow Rate : Pressure :

    Note :

    [min.]Time

    5 10 15 20

    [mV]

    Volta

    ge

    0

    100

    200

    300

    400

    500

    600

    700

    3.53

    1

    4.27

    2

    4.74

    3

    7.83

    4

    L:\ int 21140 - Unit 2 Radio

    2/25/2014 11:20 AM Page 1 of 2Chromatogram L:\int21140.PRM

  • Result Table (Uncal - L:\int21140 - Unit 2 Radio)

    CompoundName

    Reten. Time[min]

    Area[mV.s]

    Height[mV]

    Area[%]

    Height[%]

    Efficiency[th.pl]

    Eff/l[t.p./m]

    Symmetry/Tailing[-]

    Response Factor

    Resolution[-]

    1 3.53 87.540 3.05 0.46 0.44 214.58 4291.54 1.34

    2 4.27 123.887 7.10 0.65 1.04 948.06 18961.11 0.87 1.0

    3 4.74 302.210 11.28 1.58 1.65 1323.53 26470.57 2.21 0.9

    4 7.83 18599.341 663.73 97.31 96.87 2434.84 48696.74 1.63 5.4

    Total 19112.978 685.15 100.00 100.00

    2/25/2014 11:20 AM Page 2 of 2Chromatogram L:\int21140.PRM

  • MT-605Riboflavin, [3H]-

    Lot 213-021-0212-A-20090119-JG

    Chromatogram Info:

    File Name : L:\int21140 File Created : 2/25/2014 10:51:06 AM

    Origin : Acquired, Acquisition started 5/18/2011 8:52:45 AM Acquired Date : 5/18/2011 9:12:45 AM

    Project : Test By : Administrator

    Method : unit2-20minrun By : Administrator

    Description : UV trace of 3H material co-injected with standard

    Created : 8/8/2007 9:12 AM Modified : 2/25/2014 11:06 AM

    Column : Detection : UV 266nm

    Mobile Phase : Temperature :

    Flow Rate : Pressure :

    Note :

    [min.]Time

    5 10 15 20

    [mV]

    Volta

    ge

    0

    100

    200

    300

    400

    4.48

    1

    5.19

    2

    7.62

    3

    8.35

    4

    9.22

    5

    9.66

    6

    L:\ int 21140 - Unit 2 UV

    2/25/2014 11:06 AM Page 1 of 2Chromatogram L:\int21140.PRM

  • Result Table (Uncal - L:\int21140 - Unit 2 UV)

    CompoundName

    Reten. Time[min]

    Area[mV.s]

    Height[mV]

    Area[%]

    Height[%]

    Efficiency[th.pl]

    Eff/l[t.p./m]

    Symmetry/Tailing[-]

    Response Factor

    Resolution[-]

    1 4.48 16.261 2.05 0.38 0.60 8156.91 163138.21 0.87

    2 5.19 9.685 1.03 0.22 0.30 9312.74 186254.80 0.81 3.5

    3 7.62 4261.148 335.20 98.66 98.40 9919.61 198392.23 1.32 9.3

    4 8.35 24.561 1.76 0.57 0.52 8480.44 169608.83 1.21 2.2

    5 9.22 2.935 0.27 0.07 0.08 15675.00 313499.91 0.92 2.7

    6 9.66 4.291 0.35 0.10 0.10 13840.45 276809.00 1.17 1.4

    Total 4318.880 340.66 100.00 100.00

    2/25/2014 11:06 AM Page 2 of 2Chromatogram L:\int21140.PRM

  • MT-605Riboflavin, [3H]-

    Lot 213-021-0212-A-20090119-JG

    Chromatogram Info:

    File Name : L:\int21136 File Created : 2/25/2014 10:51:06 AM

    Origin : Acquired, Acquisition started 5/17/2011 1:53:13 PM Acquired Date : 5/17/2011 2:13:13 PM

    Project : Test By : Administrator

    Method : unit2-20minrun By : Administrator

    Description : UV trace of blank injection

    Created : 8/8/2007 9:12 AM Modified : 2/25/2014 11:21 AM

    Column : Detection : UV 266nm

    Mobile Phase : Temperature :

    Flow Rate : Pressure :

    Note :

    [min.]Time

    5 10 15 20

    [mV]

    Volta

    ge

    -5

    0

    5

    10

    15

    L:\ int 21136 - Unit 2 UV

    2/25/2014 11:21 AM Page 1 of 2Chromatogram L:\int21136.PRM

  • Result Table (Uncal - L:\int21136 - Unit 2 UV)

    CompoundName

    Reten. Time[min]

    Area[mV.s]

    Height[mV]

    Area[%]

    Height[%]

    Efficiency[th.pl]

    Eff/l[t.p./m]

    Symmetry/Tailing[-]

    Response Factor

    Resolution[-]

    No peak to report

    2/25/2014 11:21 AM Page 2 of 2Chromatogram L:\int21136.PRM

  • C:\Xcalibur\data\MT605-20090119-JG 8/4/2010 11:38:12 AM MT605-20090119-JG

    RT: 0.00 - 1.99

    0.0 0.5 1.0 1.5

    Time (min)

    0

    5

    10

    15

    20

    25

    30

    35

    40

    45

    50

    55

    60

    65

    70

    75

    80

    85

    90

    95

    100

    Re

    lative

    Ab

    un

    da

    nce

    1.96

    1.731.65

    1.511.42

    1.241.130.870.510.47

    0.23

    NL:9.39E6

    TIC F: MS MT605-20090119-JG

    MT605-20090119-JG#1-157 RT: 0.00-1.99 AV:T: + c Q3MS [ 200.00-800.00]m/z= 371.57-400.28

    m/z Intensity Relativem/z Intensity Relative

    377.25 2254794.5 100.00 378.26 481660.2 21.36 379.26 548537.5 24.33 380.27 111380.5 4.94 381.27 194303.4 8.62 382.28 39598.4 1.76 383.28 174679.4 7.75 384.28 35987.5 1.60 385.29 39608.1 1.76 386.31 8305.5 0.37 387.29 33648.2 1.49 388.31 9008.4 0.40 389.30 72512.4 3.22 390.28 15106.0 0.67 391.36 14597.3 0.65 392.34 4579.3 0.20 393.28 4667.2 0.21 395.27 4999.3 0.22 399.23 43137.4 1.91 400.23 9479.1 0.42

    MT605-20090119-JG #1-157 RT: 0.00-1.99 AV: 157 NL: 2.25E6T: + c Q3MS [ 200.00-800.00]

    200 300 400 500 600 700 800

    m/z

    0

    5

    10

    15

    20

    25

    30

    35

    40

    45

    50

    55

    60

    65

    70

    75

    80

    85

    90

    95

    100

    Re

    lative

    Ab

    un

    da

    nce

    377.25

    217.26 753.35

    243.21389.30

    287.30 469.31 593.25 634.98

    MT605-20090119-JG #1-157 RT: 0.00-1.99 AV: 157 NL: 2.25E6T: + c Q3MS [ 200.00-800.00]

    360 380 400 420 440

    m/z

    0

    5

    10

    15

    20

    25

    30

    35

    40

    45

    50

    55

    60

    65

    70

    75

    80

    85

    90

    95

    100

    Re

    lative

    Ab

    un

    da

    nce

    377.25

    379.26

    381.27

    389.30399.23 411.26 455.29423.30371.32 445.28

  • 98

    76

    54

    32

    1pp

    m

    2.3142.4172.4672.523

    1.00

    PC 1.00

    GB 0

    LB 0.00 Hz

    SSB 0

    WDW no

    SF 320.1305850 MHz

    SI 32768

    SFO1 320.1321857 MHz

    PL1 2.00 dB

    P1 10.00 usec

    NUC1 3H

    ======== CHANNEL f1 ========

    TD0 1

    D1 2.00000000 sec

    TE 300.0 K

    DE 6.00 usec

    DW 81.000 usec

    RG 46341

    AQ 1.3271540 sec

    FIDRES 0.376760 Hz

    SWH 6172.839 Hz

    DS 2

    NS 5000

    SOLVENT D2O

    TD 16384

    PULPROG zg

    PROBHD 5 mm DUX 3H−1H

    INSTRUM spect

    Time 15.20

    Date_ 20110520

    PROCNO 1

    EXPNO 2

    NAME MT605−20090119−JG

    Batch 20090119−JG

    MT605 3H NMR in D2O

    Table of contents for MT605 Lot 213-021-0212-A-20090119-JGint21138radint21138uvint21139uvStdint21140radCoint21140uvCoint21136uvBlkMT605-20090119-JG-MS-2mt605-20090119-jg-nmr-1