chromatograph - hplc.sk · chromatograph think about food care about safety macherey-nagel gmbh...

8
CHROMATOGRAPHY Think about food Care about safety www.mn-net.com Vol. 7 Pesticides

Upload: vodang

Post on 10-Sep-2018

216 views

Category:

Documents


0 download

TRANSCRIPT

Page 1: CHROMATOGRAPH - hplc.sk · CHROMATOGRAPH Think about food Care about safety  MACHEREY-NAGEL GmbH & Co. KG · Neumann-Neander-Str. 6 8 · 52355 Düren · Deutschland  Frankreich:

CHROMATOGRAPHY

Think about foodCare about safety

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL GmbH amp Co KG middot Neumann-Neander-Str 6ndash8 middot 52355 Duumlren middot DeutschlandFrankreichMACHEREY-NAGEL EURLTel +33 388 68 22 68Fax +33 388 51 76 88E-Mail sales-frmn-netcom

SchweizMACHEREY-NAGEL AGTel +41 62 388 55 00Fax +41 62 388 55 05E-Mail sales-chmn-netcom

Deutschlandund InternationalTel +49 24 21 969-0Fax +49 24 21 969-199E-Mail infomn-netcom

MACHEREY-NAGEL

EN ISO 9001 2008ZERTIFIZIERT

USAMACHEREY-NAGEL IncTel +1 484 821 0984Fax +1 484 821 1272E-Mail sales-usmn-netcom

Vol 7Pesticides

infomn-netcom wwwmn-netcom2 3

Focus on pesticides The global production and trading of food and feed products makes monitoring and control difficult

Only analysis of food and raw materials for the production of food can ensure safe and edible food Food safety is an essential part of our quality of life

MN shows examples for food analysis that will help you with your work and make our food safer

Vol 7 Pesticides in foodPesticides are chemical agents used for prevention and control of various pests Pesticides can be classified in herbicides (to control weeds) insecticides (to control in-sects) fungicides (to control molds and fungi) and roden-ticides (to control rodents) [EPA ndash US Environmental Protec-tion Agency ndash httpwwwepagovpesticidesfood]

Most commonly used are

bullOrganophosphates

bullCarbamates

bullPyrethroids

bullSulfonylurea

bullGlyphosate

bullOrganochlorine compounds

Since pesticides can be harmful to health of humans an-imals or the environment they need to be monitored and very responsibly used [EPA ndash US Environmental Protection Agency ndash httpwwwepagovpesticideshealthhumanhtm]

Among other authorities the US Environmental Protec-tion Agency (EPA) sets limits on how much of a pesticide can be used on food during the growing and processing and how much is allowed to remain in the food [EPA ndash US Environmental Protection Agency ndash httpwwwepagovpesti-cidessafetyapplicatorsrestricthtm]

infomn-netcom wwwmn-netcom2 3

Compounds of interestChemical structures of selected pesticides

Dioxathion Dimethoate Glyphosate Chlorpyriphos Chlorfenvinphos

PP

OC2H5H5C2O

OC2H5H5C2O

SS

SS

OO

PH3CO

OCH3

SSN

H

OH3C

OOP

HN OHHO

HO

PH5C2O

OC2H5

SO

N

Cl

Cl

Cl

Cl

Cl

O

OPO O

Cl

CH3

CH3

Propamocarb Carbaryl Carbofuran Aldicarb Pirimicarb

NH

OCH3

CH3

N OH3C NHO

OCH3

O CH3CH3

NHO

OCH3

CH3CH3

NNH ndash CH3O

O

H3C ndash S N(CH3)2

NN

H3C

H3C

N(CH3)2O

O

Diuron Linuron Metoxuron Chlortoluron Pencycuron

Cl

Cl O

NHN(CH3)2 H

N NO

CH3

OCH3Cl

Cl

HN N

O

CH3

CH3Cl

H3CO

HN N

O

CH3

CH3Cl

H3C O

NHN

Cl

Endosulfan Heptachlor Nonachlor Aldrin EndrinClCl

ClCl

ClCl

O = SO

O

ClClCl

Cl

ClClCl

ClCl

Cl

ClCl

ClClCl

ClClCl

ClCl

ClCl

ClClCl

Cl

ClCl

O

Actochlor Metholachlor 44rsquo-DDD 44rsquo-DDE 44rsquo-DDT

NO

O

CH3

CH3C2H5

CH2ClCl

O CH3OCH3

C2H5H3CN

Cl Cl

CHCl2

Cl Cl

CCl2

Cl Cl

CCl3

Difenoconazol Cyproconazol Fenbuconazole Paclobutrazol MetazachlorH3C

NCl Cl

NN

O O

O

OH

CH3

Cl

N NN

NNN

Cl

NC

CH3

CH3

CH3OH

NNN

ClCl

O N NN

H3C CH3

Triazines

NN N

R2 R3

R1 Compound R1 R2 R3

Atrazine Cl NH-C2H5 NH-CH(CH3)2Simazine Cl NH-C2H5 NH-C2H5Terbuthylazine Cl NH-C2H5 NH-C(CH3)3Terbutryn S-CH3 NH-C2H5 NH-C(CH3)3

infomn-netcom wwwmn-netcom4 5

Typical samples preparation Pesticides from natural water

MN AAp MNo 305520

c Column type CHROMABONDreg HR-X 3 mL 60 mg REF 730936

Column conditioning 5 mL methanol then 5 mL ultrapure waterSample aspiration 50 mL water sample is passed through the column by vacuumWashing 5 mL ultrapure water with 5 methanolDrying with gentle nitrogen stream 15 min (storage before elution step at 4 degC is possible for 1 month)Elution 2 x 3 mL methanol then 1 x 3 mL methanol ndash ethyl acetate (7525 vv)Evaporation to dryness after addition of 10 μL internal standardReconstitution in 1 mL of the initial HPLC eluent

Compounds investigated acetochlor alachlor atrazine azoxystrobin carbaryl carbo-furan 3-hydroxycarbofuran chlorfenvinphos chlorpyriphos chlortoluron 1-(34-dichlorophenyl)-3-methyl urea (DCPMU metabolite of diuron) desethylatrazine (DEA metabolite of atrazine) desethylterbuthylazine (DET metabolite of terbuth-ylazine) desisopropylatrazine (DIA metabolite of atrazine) dimethoate dimetomorph diuron hexazinone 1-(4-isopro-pylphenyl)-3-methyl urea (IPPMU metabolite of isoproturon) 1-(4-isopropyl phenyl) urea (IPPU metabolite of isoproturon) isoproturon linuron metazachlor methomyl metolachlor metoxuron pyrimicarb simazine terbuthylazine thiodicarb

We recommend using the CHROMABONDreg vacuum manifold for 12 columns REF 730150

Pesticide residues from fruit and vegetables using the QuEChERS procedureMN AAp MNo 305190

c Column type CHROMABONDreg QuEChERS Mix I REF 730970 CHROMABONDreg QuEChERS Mix III REF 730972

Sample pretreatment The food sample is homogenized in a 50 mL centrifuge tube (REF 730223) with 8 mL acetonitrile and then cleaned up with pre-weighed mixes of salts and adsorbents in a 15 mL centrifuge tubeProcedure for complex food samples The sample is extracted with Mix I then 1 mL supernantant is transferred to the centrifuge tube with Mix III (samples with low fat content) It is shaken centrifuged and analyzed by HPLC Compounds investigated aldicarb sulfone aldicarb desmethyl-pirimicarb desmethyl-formamido-pirimicarb carbofuran paclobutrazol terbutryn pencycuron dioxathion fenpyroximate oxamyl pymetrozin propamocarb dimethoate carbendazim metalaxyl methoxy-fenozide tebufenozide fenoxycarb pyraclostrobin difeno-conazol propargite spinosad methiocarb sulfoxide thio-phanate-m dimethomorph I fludioxonil fenbuconazol famoxadone prosulfocarb dimethomorph II cyproconazol I cyproconazol II hydroxycarbofuran

Transfer into a sample vial eg 15 mL screw neck vials N 9 amber flat bottom label and scale wide opening REF 702284 and ready assembled screw closures N 9 blue center hole with septum silicone PTFE REF 7022871 11

6 x

32

mm

For other applications see wwwmn-netcomaAAs

infomn-netcom wwwmn-netcom4 5

Sample preparation and analysis Fungicides carbendazime and thiabendazole from fruit juiceSolid phase extraction

MN AAp MNo 304740Sample pretreatment see wwwmn-netcomaAAs

c Column type CHROMABONDreg HR-XC 3 mL 200 mg REF 730952

Column conditioning 5 mL methanol then 5 mL 2 NH3 (Do not let run the column dry)Sample aspiration The prepared sample is passed through the column by vacuumWashing impurities are removed with the following washing mixtures a) 2 mL 2 NH3 b) 2 mL 30 methanol ndash 5 NH3 c) 2 mL 01 molL HCl d) 2 mL methanolDrying with nitrogen or airElution 4 mL methanol 5 NH3

It is recommended to filter the prepared sample through dis-posable filters CHROMAFILreg Xtra PET-4525 REF 729220

HPLC analysisMN AAp MNo 122200

Column EC 1254 NUCLEODURreg C18 Gravity 5 μm REF 76010040

0 2 4 6 8 10 min

2

1

Peaks1 Carbendazime

OCH3NH

NHN

O2 ThiabendazoleNN

S NH

Detailed conditions are available online at wwwmn-netcomaAAs

MN suggests using guard columns to protect your main column and significantly increase column life

The Column Protection System (REF 718966) is suitable for all analytical HPLC columns with 116 fittings

infomn-netcom wwwmn-netcom6 7

Analysis Subsequent analysis GCPesticides from cod liver oil

MN AAp MNo 213270R Looser K Ballschmiter J Chromatogr A 836 271ndash284 (1999)Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film

REF 72642060

1

4

2

7

8

9

10

11

12

13

1415

16

1719

20

21

2223

24

2527

30

31

33

3432

29

26 2818

3 4

5

6

10 20 30 40 50min

b)

a)

It is recommended to filter the prepared sample through disposable filters CHROMAFILreg PTFE-4525 REF 729205

Organochlorine pesticides (EPA 8081)MN AAp MNo 213630

Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film REF 72616230

Peaks1 2456-Tetrachloro-

m-xylene2 α-BHC3 γ-BHC (Lindane)4 Heptachlor5 β-BHC6 Aldrin7 δ-BHC8 Heptachlor epoxide9 γ-Chlordane10 α-Chlordane11 Endosulfan I

12 44-DDE13 Dieldrin14 Endrin15 44-DDD16 Endosulfan II17 44-DDT18 Endrin aldehyde19 Endosulfan sulfate20 Methoxychlor21 Endrin ketone22 Decachlorobiphenyl

Detailed conditions are available on-line at wwwmn-netcomaAAs

Peaks1 Pentachlorobenzene2 246-Tribromoanisole3 Tetrachloro-14-dimethoxy-

benzene4 α-BHC5 Pentachloroanisole6 HCB7 γ-BHC8 β-BHC9 Heptachlor10 ε-BHC11 Aldrin12 1234-Tetrachloro-

naphthalene (TCN)13 PCB-10314 Oxychlordane15 cis-Heptachlor epoxide

16 24-DDE17 trans-Chlordane18 cis-Chlordane

trans-Nonachlor19 Endosulfan I20 44-DDE21 Dieldrin22 24-DDD23 Endrin24 24-DDT25 cis-Nonachlor26 44-DDD27 Endosulfan II28 44-DDT29 Parlar 4130 Parlar 4031 Parlar 4432 Endosulfan sulphate33 Parlar 5034 Mirex

1

2

3

4

5

6

7 8

9 10

11

12

1314

15

17

18

1920

21

2216

64 12108 14 min

infomn-netcom wwwmn-netcom6 7

Product information Ordering informationStep Product Pack of REFSPE 1 CHROMABONDreg HR-X 3 mL 60 mg 30 730936

CHROMABONDreg vacuum manifold for 12 columns 1 730150SPE 2 (QuEChERS) CHROMABONDreg QuEChERS Mix I (citrate extraction mix) 50 730970

CHROMABONDreg QuEChERS Mix III (Diamino clean-up mix) 50 730972SPE 3 CHROMABONDreg HR-XC 3 mL 200 mg 30 730952

CHROMABONDreg vacuum manifold for 12 columns 1 730150Filtration Disposable filters CHROMAFILreg Xtra PET-4525 100 729220

Disposable filters CHROMAFILreg Xtra PTFE-4525 100 729205Vials and caps 15 mL screw neck vials N 9 amber label and scale 100 702284

Ready assembled screw closures N 9 blue center hole with septum Silicone white PTFE red

100 7022871

HPLCColumn EC 1254 NUCLEODURreg C18 Gravity 5 μm 1 76010040Guard column EC 43 NUCLEODURreg C18 Gravity 5 μm 3 76190330Guard column holder Column Protection System 1 718966GC 1Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film 1 72642060GC 2Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film 1 72616230

Visit us at wwwmn-netcomchroma to get more helpful information

Selection tools for

Vials and caps

Syringe filters

Troubleshooting guidesGC and HPLC

Detailed product information

hellipand much more

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL

EN ISO 9001 2008CERTIFIED

Food safety made easy with products from

MACHEREY-NAGEL

Vol 8

Additives

Vol 6

Mycotoxins

Vol 2

Vitamins

Vol 4

Acrylamide

Vol 1

Melamine

Vol 5

Sugars Sweeteners

Vol 3

AntibioticsVol 7

Pesticides

KATE

N20

0123

Foc

us F

lyer

Foo

d Vo

l 7

en1

10

031

5 PD

Pr

inte

d in

Ger

man

yIm

age

cred

its copy

Tija

na o

lga

dem

schi

shin

a P

ierre

bril

lot

Pete

r Her

mes

Fur

ian

ar

enaf

otou

k fo

vito

nic

eday

rr1

45 a

irbor

ne77

Sl

y SA

DEQ

ndash fo

tolia

com

Page 2: CHROMATOGRAPH - hplc.sk · CHROMATOGRAPH Think about food Care about safety  MACHEREY-NAGEL GmbH & Co. KG · Neumann-Neander-Str. 6 8 · 52355 Düren · Deutschland  Frankreich:

infomn-netcom wwwmn-netcom2 3

Focus on pesticides The global production and trading of food and feed products makes monitoring and control difficult

Only analysis of food and raw materials for the production of food can ensure safe and edible food Food safety is an essential part of our quality of life

MN shows examples for food analysis that will help you with your work and make our food safer

Vol 7 Pesticides in foodPesticides are chemical agents used for prevention and control of various pests Pesticides can be classified in herbicides (to control weeds) insecticides (to control in-sects) fungicides (to control molds and fungi) and roden-ticides (to control rodents) [EPA ndash US Environmental Protec-tion Agency ndash httpwwwepagovpesticidesfood]

Most commonly used are

bullOrganophosphates

bullCarbamates

bullPyrethroids

bullSulfonylurea

bullGlyphosate

bullOrganochlorine compounds

Since pesticides can be harmful to health of humans an-imals or the environment they need to be monitored and very responsibly used [EPA ndash US Environmental Protection Agency ndash httpwwwepagovpesticideshealthhumanhtm]

Among other authorities the US Environmental Protec-tion Agency (EPA) sets limits on how much of a pesticide can be used on food during the growing and processing and how much is allowed to remain in the food [EPA ndash US Environmental Protection Agency ndash httpwwwepagovpesti-cidessafetyapplicatorsrestricthtm]

infomn-netcom wwwmn-netcom2 3

Compounds of interestChemical structures of selected pesticides

Dioxathion Dimethoate Glyphosate Chlorpyriphos Chlorfenvinphos

PP

OC2H5H5C2O

OC2H5H5C2O

SS

SS

OO

PH3CO

OCH3

SSN

H

OH3C

OOP

HN OHHO

HO

PH5C2O

OC2H5

SO

N

Cl

Cl

Cl

Cl

Cl

O

OPO O

Cl

CH3

CH3

Propamocarb Carbaryl Carbofuran Aldicarb Pirimicarb

NH

OCH3

CH3

N OH3C NHO

OCH3

O CH3CH3

NHO

OCH3

CH3CH3

NNH ndash CH3O

O

H3C ndash S N(CH3)2

NN

H3C

H3C

N(CH3)2O

O

Diuron Linuron Metoxuron Chlortoluron Pencycuron

Cl

Cl O

NHN(CH3)2 H

N NO

CH3

OCH3Cl

Cl

HN N

O

CH3

CH3Cl

H3CO

HN N

O

CH3

CH3Cl

H3C O

NHN

Cl

Endosulfan Heptachlor Nonachlor Aldrin EndrinClCl

ClCl

ClCl

O = SO

O

ClClCl

Cl

ClClCl

ClCl

Cl

ClCl

ClClCl

ClClCl

ClCl

ClCl

ClClCl

Cl

ClCl

O

Actochlor Metholachlor 44rsquo-DDD 44rsquo-DDE 44rsquo-DDT

NO

O

CH3

CH3C2H5

CH2ClCl

O CH3OCH3

C2H5H3CN

Cl Cl

CHCl2

Cl Cl

CCl2

Cl Cl

CCl3

Difenoconazol Cyproconazol Fenbuconazole Paclobutrazol MetazachlorH3C

NCl Cl

NN

O O

O

OH

CH3

Cl

N NN

NNN

Cl

NC

CH3

CH3

CH3OH

NNN

ClCl

O N NN

H3C CH3

Triazines

NN N

R2 R3

R1 Compound R1 R2 R3

Atrazine Cl NH-C2H5 NH-CH(CH3)2Simazine Cl NH-C2H5 NH-C2H5Terbuthylazine Cl NH-C2H5 NH-C(CH3)3Terbutryn S-CH3 NH-C2H5 NH-C(CH3)3

infomn-netcom wwwmn-netcom4 5

Typical samples preparation Pesticides from natural water

MN AAp MNo 305520

c Column type CHROMABONDreg HR-X 3 mL 60 mg REF 730936

Column conditioning 5 mL methanol then 5 mL ultrapure waterSample aspiration 50 mL water sample is passed through the column by vacuumWashing 5 mL ultrapure water with 5 methanolDrying with gentle nitrogen stream 15 min (storage before elution step at 4 degC is possible for 1 month)Elution 2 x 3 mL methanol then 1 x 3 mL methanol ndash ethyl acetate (7525 vv)Evaporation to dryness after addition of 10 μL internal standardReconstitution in 1 mL of the initial HPLC eluent

Compounds investigated acetochlor alachlor atrazine azoxystrobin carbaryl carbo-furan 3-hydroxycarbofuran chlorfenvinphos chlorpyriphos chlortoluron 1-(34-dichlorophenyl)-3-methyl urea (DCPMU metabolite of diuron) desethylatrazine (DEA metabolite of atrazine) desethylterbuthylazine (DET metabolite of terbuth-ylazine) desisopropylatrazine (DIA metabolite of atrazine) dimethoate dimetomorph diuron hexazinone 1-(4-isopro-pylphenyl)-3-methyl urea (IPPMU metabolite of isoproturon) 1-(4-isopropyl phenyl) urea (IPPU metabolite of isoproturon) isoproturon linuron metazachlor methomyl metolachlor metoxuron pyrimicarb simazine terbuthylazine thiodicarb

We recommend using the CHROMABONDreg vacuum manifold for 12 columns REF 730150

Pesticide residues from fruit and vegetables using the QuEChERS procedureMN AAp MNo 305190

c Column type CHROMABONDreg QuEChERS Mix I REF 730970 CHROMABONDreg QuEChERS Mix III REF 730972

Sample pretreatment The food sample is homogenized in a 50 mL centrifuge tube (REF 730223) with 8 mL acetonitrile and then cleaned up with pre-weighed mixes of salts and adsorbents in a 15 mL centrifuge tubeProcedure for complex food samples The sample is extracted with Mix I then 1 mL supernantant is transferred to the centrifuge tube with Mix III (samples with low fat content) It is shaken centrifuged and analyzed by HPLC Compounds investigated aldicarb sulfone aldicarb desmethyl-pirimicarb desmethyl-formamido-pirimicarb carbofuran paclobutrazol terbutryn pencycuron dioxathion fenpyroximate oxamyl pymetrozin propamocarb dimethoate carbendazim metalaxyl methoxy-fenozide tebufenozide fenoxycarb pyraclostrobin difeno-conazol propargite spinosad methiocarb sulfoxide thio-phanate-m dimethomorph I fludioxonil fenbuconazol famoxadone prosulfocarb dimethomorph II cyproconazol I cyproconazol II hydroxycarbofuran

Transfer into a sample vial eg 15 mL screw neck vials N 9 amber flat bottom label and scale wide opening REF 702284 and ready assembled screw closures N 9 blue center hole with septum silicone PTFE REF 7022871 11

6 x

32

mm

For other applications see wwwmn-netcomaAAs

infomn-netcom wwwmn-netcom4 5

Sample preparation and analysis Fungicides carbendazime and thiabendazole from fruit juiceSolid phase extraction

MN AAp MNo 304740Sample pretreatment see wwwmn-netcomaAAs

c Column type CHROMABONDreg HR-XC 3 mL 200 mg REF 730952

Column conditioning 5 mL methanol then 5 mL 2 NH3 (Do not let run the column dry)Sample aspiration The prepared sample is passed through the column by vacuumWashing impurities are removed with the following washing mixtures a) 2 mL 2 NH3 b) 2 mL 30 methanol ndash 5 NH3 c) 2 mL 01 molL HCl d) 2 mL methanolDrying with nitrogen or airElution 4 mL methanol 5 NH3

It is recommended to filter the prepared sample through dis-posable filters CHROMAFILreg Xtra PET-4525 REF 729220

HPLC analysisMN AAp MNo 122200

Column EC 1254 NUCLEODURreg C18 Gravity 5 μm REF 76010040

0 2 4 6 8 10 min

2

1

Peaks1 Carbendazime

OCH3NH

NHN

O2 ThiabendazoleNN

S NH

Detailed conditions are available online at wwwmn-netcomaAAs

MN suggests using guard columns to protect your main column and significantly increase column life

The Column Protection System (REF 718966) is suitable for all analytical HPLC columns with 116 fittings

infomn-netcom wwwmn-netcom6 7

Analysis Subsequent analysis GCPesticides from cod liver oil

MN AAp MNo 213270R Looser K Ballschmiter J Chromatogr A 836 271ndash284 (1999)Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film

REF 72642060

1

4

2

7

8

9

10

11

12

13

1415

16

1719

20

21

2223

24

2527

30

31

33

3432

29

26 2818

3 4

5

6

10 20 30 40 50min

b)

a)

It is recommended to filter the prepared sample through disposable filters CHROMAFILreg PTFE-4525 REF 729205

Organochlorine pesticides (EPA 8081)MN AAp MNo 213630

Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film REF 72616230

Peaks1 2456-Tetrachloro-

m-xylene2 α-BHC3 γ-BHC (Lindane)4 Heptachlor5 β-BHC6 Aldrin7 δ-BHC8 Heptachlor epoxide9 γ-Chlordane10 α-Chlordane11 Endosulfan I

12 44-DDE13 Dieldrin14 Endrin15 44-DDD16 Endosulfan II17 44-DDT18 Endrin aldehyde19 Endosulfan sulfate20 Methoxychlor21 Endrin ketone22 Decachlorobiphenyl

Detailed conditions are available on-line at wwwmn-netcomaAAs

Peaks1 Pentachlorobenzene2 246-Tribromoanisole3 Tetrachloro-14-dimethoxy-

benzene4 α-BHC5 Pentachloroanisole6 HCB7 γ-BHC8 β-BHC9 Heptachlor10 ε-BHC11 Aldrin12 1234-Tetrachloro-

naphthalene (TCN)13 PCB-10314 Oxychlordane15 cis-Heptachlor epoxide

16 24-DDE17 trans-Chlordane18 cis-Chlordane

trans-Nonachlor19 Endosulfan I20 44-DDE21 Dieldrin22 24-DDD23 Endrin24 24-DDT25 cis-Nonachlor26 44-DDD27 Endosulfan II28 44-DDT29 Parlar 4130 Parlar 4031 Parlar 4432 Endosulfan sulphate33 Parlar 5034 Mirex

1

2

3

4

5

6

7 8

9 10

11

12

1314

15

17

18

1920

21

2216

64 12108 14 min

infomn-netcom wwwmn-netcom6 7

Product information Ordering informationStep Product Pack of REFSPE 1 CHROMABONDreg HR-X 3 mL 60 mg 30 730936

CHROMABONDreg vacuum manifold for 12 columns 1 730150SPE 2 (QuEChERS) CHROMABONDreg QuEChERS Mix I (citrate extraction mix) 50 730970

CHROMABONDreg QuEChERS Mix III (Diamino clean-up mix) 50 730972SPE 3 CHROMABONDreg HR-XC 3 mL 200 mg 30 730952

CHROMABONDreg vacuum manifold for 12 columns 1 730150Filtration Disposable filters CHROMAFILreg Xtra PET-4525 100 729220

Disposable filters CHROMAFILreg Xtra PTFE-4525 100 729205Vials and caps 15 mL screw neck vials N 9 amber label and scale 100 702284

Ready assembled screw closures N 9 blue center hole with septum Silicone white PTFE red

100 7022871

HPLCColumn EC 1254 NUCLEODURreg C18 Gravity 5 μm 1 76010040Guard column EC 43 NUCLEODURreg C18 Gravity 5 μm 3 76190330Guard column holder Column Protection System 1 718966GC 1Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film 1 72642060GC 2Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film 1 72616230

Visit us at wwwmn-netcomchroma to get more helpful information

Selection tools for

Vials and caps

Syringe filters

Troubleshooting guidesGC and HPLC

Detailed product information

hellipand much more

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL

EN ISO 9001 2008CERTIFIED

Food safety made easy with products from

MACHEREY-NAGEL

Vol 8

Additives

Vol 6

Mycotoxins

Vol 2

Vitamins

Vol 4

Acrylamide

Vol 1

Melamine

Vol 5

Sugars Sweeteners

Vol 3

AntibioticsVol 7

Pesticides

KATE

N20

0123

Foc

us F

lyer

Foo

d Vo

l 7

en1

10

031

5 PD

Pr

inte

d in

Ger

man

yIm

age

cred

its copy

Tija

na o

lga

dem

schi

shin

a P

ierre

bril

lot

Pete

r Her

mes

Fur

ian

ar

enaf

otou

k fo

vito

nic

eday

rr1

45 a

irbor

ne77

Sl

y SA

DEQ

ndash fo

tolia

com

Page 3: CHROMATOGRAPH - hplc.sk · CHROMATOGRAPH Think about food Care about safety  MACHEREY-NAGEL GmbH & Co. KG · Neumann-Neander-Str. 6 8 · 52355 Düren · Deutschland  Frankreich:

infomn-netcom wwwmn-netcom2 3

Compounds of interestChemical structures of selected pesticides

Dioxathion Dimethoate Glyphosate Chlorpyriphos Chlorfenvinphos

PP

OC2H5H5C2O

OC2H5H5C2O

SS

SS

OO

PH3CO

OCH3

SSN

H

OH3C

OOP

HN OHHO

HO

PH5C2O

OC2H5

SO

N

Cl

Cl

Cl

Cl

Cl

O

OPO O

Cl

CH3

CH3

Propamocarb Carbaryl Carbofuran Aldicarb Pirimicarb

NH

OCH3

CH3

N OH3C NHO

OCH3

O CH3CH3

NHO

OCH3

CH3CH3

NNH ndash CH3O

O

H3C ndash S N(CH3)2

NN

H3C

H3C

N(CH3)2O

O

Diuron Linuron Metoxuron Chlortoluron Pencycuron

Cl

Cl O

NHN(CH3)2 H

N NO

CH3

OCH3Cl

Cl

HN N

O

CH3

CH3Cl

H3CO

HN N

O

CH3

CH3Cl

H3C O

NHN

Cl

Endosulfan Heptachlor Nonachlor Aldrin EndrinClCl

ClCl

ClCl

O = SO

O

ClClCl

Cl

ClClCl

ClCl

Cl

ClCl

ClClCl

ClClCl

ClCl

ClCl

ClClCl

Cl

ClCl

O

Actochlor Metholachlor 44rsquo-DDD 44rsquo-DDE 44rsquo-DDT

NO

O

CH3

CH3C2H5

CH2ClCl

O CH3OCH3

C2H5H3CN

Cl Cl

CHCl2

Cl Cl

CCl2

Cl Cl

CCl3

Difenoconazol Cyproconazol Fenbuconazole Paclobutrazol MetazachlorH3C

NCl Cl

NN

O O

O

OH

CH3

Cl

N NN

NNN

Cl

NC

CH3

CH3

CH3OH

NNN

ClCl

O N NN

H3C CH3

Triazines

NN N

R2 R3

R1 Compound R1 R2 R3

Atrazine Cl NH-C2H5 NH-CH(CH3)2Simazine Cl NH-C2H5 NH-C2H5Terbuthylazine Cl NH-C2H5 NH-C(CH3)3Terbutryn S-CH3 NH-C2H5 NH-C(CH3)3

infomn-netcom wwwmn-netcom4 5

Typical samples preparation Pesticides from natural water

MN AAp MNo 305520

c Column type CHROMABONDreg HR-X 3 mL 60 mg REF 730936

Column conditioning 5 mL methanol then 5 mL ultrapure waterSample aspiration 50 mL water sample is passed through the column by vacuumWashing 5 mL ultrapure water with 5 methanolDrying with gentle nitrogen stream 15 min (storage before elution step at 4 degC is possible for 1 month)Elution 2 x 3 mL methanol then 1 x 3 mL methanol ndash ethyl acetate (7525 vv)Evaporation to dryness after addition of 10 μL internal standardReconstitution in 1 mL of the initial HPLC eluent

Compounds investigated acetochlor alachlor atrazine azoxystrobin carbaryl carbo-furan 3-hydroxycarbofuran chlorfenvinphos chlorpyriphos chlortoluron 1-(34-dichlorophenyl)-3-methyl urea (DCPMU metabolite of diuron) desethylatrazine (DEA metabolite of atrazine) desethylterbuthylazine (DET metabolite of terbuth-ylazine) desisopropylatrazine (DIA metabolite of atrazine) dimethoate dimetomorph diuron hexazinone 1-(4-isopro-pylphenyl)-3-methyl urea (IPPMU metabolite of isoproturon) 1-(4-isopropyl phenyl) urea (IPPU metabolite of isoproturon) isoproturon linuron metazachlor methomyl metolachlor metoxuron pyrimicarb simazine terbuthylazine thiodicarb

We recommend using the CHROMABONDreg vacuum manifold for 12 columns REF 730150

Pesticide residues from fruit and vegetables using the QuEChERS procedureMN AAp MNo 305190

c Column type CHROMABONDreg QuEChERS Mix I REF 730970 CHROMABONDreg QuEChERS Mix III REF 730972

Sample pretreatment The food sample is homogenized in a 50 mL centrifuge tube (REF 730223) with 8 mL acetonitrile and then cleaned up with pre-weighed mixes of salts and adsorbents in a 15 mL centrifuge tubeProcedure for complex food samples The sample is extracted with Mix I then 1 mL supernantant is transferred to the centrifuge tube with Mix III (samples with low fat content) It is shaken centrifuged and analyzed by HPLC Compounds investigated aldicarb sulfone aldicarb desmethyl-pirimicarb desmethyl-formamido-pirimicarb carbofuran paclobutrazol terbutryn pencycuron dioxathion fenpyroximate oxamyl pymetrozin propamocarb dimethoate carbendazim metalaxyl methoxy-fenozide tebufenozide fenoxycarb pyraclostrobin difeno-conazol propargite spinosad methiocarb sulfoxide thio-phanate-m dimethomorph I fludioxonil fenbuconazol famoxadone prosulfocarb dimethomorph II cyproconazol I cyproconazol II hydroxycarbofuran

Transfer into a sample vial eg 15 mL screw neck vials N 9 amber flat bottom label and scale wide opening REF 702284 and ready assembled screw closures N 9 blue center hole with septum silicone PTFE REF 7022871 11

6 x

32

mm

For other applications see wwwmn-netcomaAAs

infomn-netcom wwwmn-netcom4 5

Sample preparation and analysis Fungicides carbendazime and thiabendazole from fruit juiceSolid phase extraction

MN AAp MNo 304740Sample pretreatment see wwwmn-netcomaAAs

c Column type CHROMABONDreg HR-XC 3 mL 200 mg REF 730952

Column conditioning 5 mL methanol then 5 mL 2 NH3 (Do not let run the column dry)Sample aspiration The prepared sample is passed through the column by vacuumWashing impurities are removed with the following washing mixtures a) 2 mL 2 NH3 b) 2 mL 30 methanol ndash 5 NH3 c) 2 mL 01 molL HCl d) 2 mL methanolDrying with nitrogen or airElution 4 mL methanol 5 NH3

It is recommended to filter the prepared sample through dis-posable filters CHROMAFILreg Xtra PET-4525 REF 729220

HPLC analysisMN AAp MNo 122200

Column EC 1254 NUCLEODURreg C18 Gravity 5 μm REF 76010040

0 2 4 6 8 10 min

2

1

Peaks1 Carbendazime

OCH3NH

NHN

O2 ThiabendazoleNN

S NH

Detailed conditions are available online at wwwmn-netcomaAAs

MN suggests using guard columns to protect your main column and significantly increase column life

The Column Protection System (REF 718966) is suitable for all analytical HPLC columns with 116 fittings

infomn-netcom wwwmn-netcom6 7

Analysis Subsequent analysis GCPesticides from cod liver oil

MN AAp MNo 213270R Looser K Ballschmiter J Chromatogr A 836 271ndash284 (1999)Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film

REF 72642060

1

4

2

7

8

9

10

11

12

13

1415

16

1719

20

21

2223

24

2527

30

31

33

3432

29

26 2818

3 4

5

6

10 20 30 40 50min

b)

a)

It is recommended to filter the prepared sample through disposable filters CHROMAFILreg PTFE-4525 REF 729205

Organochlorine pesticides (EPA 8081)MN AAp MNo 213630

Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film REF 72616230

Peaks1 2456-Tetrachloro-

m-xylene2 α-BHC3 γ-BHC (Lindane)4 Heptachlor5 β-BHC6 Aldrin7 δ-BHC8 Heptachlor epoxide9 γ-Chlordane10 α-Chlordane11 Endosulfan I

12 44-DDE13 Dieldrin14 Endrin15 44-DDD16 Endosulfan II17 44-DDT18 Endrin aldehyde19 Endosulfan sulfate20 Methoxychlor21 Endrin ketone22 Decachlorobiphenyl

Detailed conditions are available on-line at wwwmn-netcomaAAs

Peaks1 Pentachlorobenzene2 246-Tribromoanisole3 Tetrachloro-14-dimethoxy-

benzene4 α-BHC5 Pentachloroanisole6 HCB7 γ-BHC8 β-BHC9 Heptachlor10 ε-BHC11 Aldrin12 1234-Tetrachloro-

naphthalene (TCN)13 PCB-10314 Oxychlordane15 cis-Heptachlor epoxide

16 24-DDE17 trans-Chlordane18 cis-Chlordane

trans-Nonachlor19 Endosulfan I20 44-DDE21 Dieldrin22 24-DDD23 Endrin24 24-DDT25 cis-Nonachlor26 44-DDD27 Endosulfan II28 44-DDT29 Parlar 4130 Parlar 4031 Parlar 4432 Endosulfan sulphate33 Parlar 5034 Mirex

1

2

3

4

5

6

7 8

9 10

11

12

1314

15

17

18

1920

21

2216

64 12108 14 min

infomn-netcom wwwmn-netcom6 7

Product information Ordering informationStep Product Pack of REFSPE 1 CHROMABONDreg HR-X 3 mL 60 mg 30 730936

CHROMABONDreg vacuum manifold for 12 columns 1 730150SPE 2 (QuEChERS) CHROMABONDreg QuEChERS Mix I (citrate extraction mix) 50 730970

CHROMABONDreg QuEChERS Mix III (Diamino clean-up mix) 50 730972SPE 3 CHROMABONDreg HR-XC 3 mL 200 mg 30 730952

CHROMABONDreg vacuum manifold for 12 columns 1 730150Filtration Disposable filters CHROMAFILreg Xtra PET-4525 100 729220

Disposable filters CHROMAFILreg Xtra PTFE-4525 100 729205Vials and caps 15 mL screw neck vials N 9 amber label and scale 100 702284

Ready assembled screw closures N 9 blue center hole with septum Silicone white PTFE red

100 7022871

HPLCColumn EC 1254 NUCLEODURreg C18 Gravity 5 μm 1 76010040Guard column EC 43 NUCLEODURreg C18 Gravity 5 μm 3 76190330Guard column holder Column Protection System 1 718966GC 1Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film 1 72642060GC 2Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film 1 72616230

Visit us at wwwmn-netcomchroma to get more helpful information

Selection tools for

Vials and caps

Syringe filters

Troubleshooting guidesGC and HPLC

Detailed product information

hellipand much more

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL

EN ISO 9001 2008CERTIFIED

Food safety made easy with products from

MACHEREY-NAGEL

Vol 8

Additives

Vol 6

Mycotoxins

Vol 2

Vitamins

Vol 4

Acrylamide

Vol 1

Melamine

Vol 5

Sugars Sweeteners

Vol 3

AntibioticsVol 7

Pesticides

KATE

N20

0123

Foc

us F

lyer

Foo

d Vo

l 7

en1

10

031

5 PD

Pr

inte

d in

Ger

man

yIm

age

cred

its copy

Tija

na o

lga

dem

schi

shin

a P

ierre

bril

lot

Pete

r Her

mes

Fur

ian

ar

enaf

otou

k fo

vito

nic

eday

rr1

45 a

irbor

ne77

Sl

y SA

DEQ

ndash fo

tolia

com

Page 4: CHROMATOGRAPH - hplc.sk · CHROMATOGRAPH Think about food Care about safety  MACHEREY-NAGEL GmbH & Co. KG · Neumann-Neander-Str. 6 8 · 52355 Düren · Deutschland  Frankreich:

infomn-netcom wwwmn-netcom4 5

Typical samples preparation Pesticides from natural water

MN AAp MNo 305520

c Column type CHROMABONDreg HR-X 3 mL 60 mg REF 730936

Column conditioning 5 mL methanol then 5 mL ultrapure waterSample aspiration 50 mL water sample is passed through the column by vacuumWashing 5 mL ultrapure water with 5 methanolDrying with gentle nitrogen stream 15 min (storage before elution step at 4 degC is possible for 1 month)Elution 2 x 3 mL methanol then 1 x 3 mL methanol ndash ethyl acetate (7525 vv)Evaporation to dryness after addition of 10 μL internal standardReconstitution in 1 mL of the initial HPLC eluent

Compounds investigated acetochlor alachlor atrazine azoxystrobin carbaryl carbo-furan 3-hydroxycarbofuran chlorfenvinphos chlorpyriphos chlortoluron 1-(34-dichlorophenyl)-3-methyl urea (DCPMU metabolite of diuron) desethylatrazine (DEA metabolite of atrazine) desethylterbuthylazine (DET metabolite of terbuth-ylazine) desisopropylatrazine (DIA metabolite of atrazine) dimethoate dimetomorph diuron hexazinone 1-(4-isopro-pylphenyl)-3-methyl urea (IPPMU metabolite of isoproturon) 1-(4-isopropyl phenyl) urea (IPPU metabolite of isoproturon) isoproturon linuron metazachlor methomyl metolachlor metoxuron pyrimicarb simazine terbuthylazine thiodicarb

We recommend using the CHROMABONDreg vacuum manifold for 12 columns REF 730150

Pesticide residues from fruit and vegetables using the QuEChERS procedureMN AAp MNo 305190

c Column type CHROMABONDreg QuEChERS Mix I REF 730970 CHROMABONDreg QuEChERS Mix III REF 730972

Sample pretreatment The food sample is homogenized in a 50 mL centrifuge tube (REF 730223) with 8 mL acetonitrile and then cleaned up with pre-weighed mixes of salts and adsorbents in a 15 mL centrifuge tubeProcedure for complex food samples The sample is extracted with Mix I then 1 mL supernantant is transferred to the centrifuge tube with Mix III (samples with low fat content) It is shaken centrifuged and analyzed by HPLC Compounds investigated aldicarb sulfone aldicarb desmethyl-pirimicarb desmethyl-formamido-pirimicarb carbofuran paclobutrazol terbutryn pencycuron dioxathion fenpyroximate oxamyl pymetrozin propamocarb dimethoate carbendazim metalaxyl methoxy-fenozide tebufenozide fenoxycarb pyraclostrobin difeno-conazol propargite spinosad methiocarb sulfoxide thio-phanate-m dimethomorph I fludioxonil fenbuconazol famoxadone prosulfocarb dimethomorph II cyproconazol I cyproconazol II hydroxycarbofuran

Transfer into a sample vial eg 15 mL screw neck vials N 9 amber flat bottom label and scale wide opening REF 702284 and ready assembled screw closures N 9 blue center hole with septum silicone PTFE REF 7022871 11

6 x

32

mm

For other applications see wwwmn-netcomaAAs

infomn-netcom wwwmn-netcom4 5

Sample preparation and analysis Fungicides carbendazime and thiabendazole from fruit juiceSolid phase extraction

MN AAp MNo 304740Sample pretreatment see wwwmn-netcomaAAs

c Column type CHROMABONDreg HR-XC 3 mL 200 mg REF 730952

Column conditioning 5 mL methanol then 5 mL 2 NH3 (Do not let run the column dry)Sample aspiration The prepared sample is passed through the column by vacuumWashing impurities are removed with the following washing mixtures a) 2 mL 2 NH3 b) 2 mL 30 methanol ndash 5 NH3 c) 2 mL 01 molL HCl d) 2 mL methanolDrying with nitrogen or airElution 4 mL methanol 5 NH3

It is recommended to filter the prepared sample through dis-posable filters CHROMAFILreg Xtra PET-4525 REF 729220

HPLC analysisMN AAp MNo 122200

Column EC 1254 NUCLEODURreg C18 Gravity 5 μm REF 76010040

0 2 4 6 8 10 min

2

1

Peaks1 Carbendazime

OCH3NH

NHN

O2 ThiabendazoleNN

S NH

Detailed conditions are available online at wwwmn-netcomaAAs

MN suggests using guard columns to protect your main column and significantly increase column life

The Column Protection System (REF 718966) is suitable for all analytical HPLC columns with 116 fittings

infomn-netcom wwwmn-netcom6 7

Analysis Subsequent analysis GCPesticides from cod liver oil

MN AAp MNo 213270R Looser K Ballschmiter J Chromatogr A 836 271ndash284 (1999)Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film

REF 72642060

1

4

2

7

8

9

10

11

12

13

1415

16

1719

20

21

2223

24

2527

30

31

33

3432

29

26 2818

3 4

5

6

10 20 30 40 50min

b)

a)

It is recommended to filter the prepared sample through disposable filters CHROMAFILreg PTFE-4525 REF 729205

Organochlorine pesticides (EPA 8081)MN AAp MNo 213630

Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film REF 72616230

Peaks1 2456-Tetrachloro-

m-xylene2 α-BHC3 γ-BHC (Lindane)4 Heptachlor5 β-BHC6 Aldrin7 δ-BHC8 Heptachlor epoxide9 γ-Chlordane10 α-Chlordane11 Endosulfan I

12 44-DDE13 Dieldrin14 Endrin15 44-DDD16 Endosulfan II17 44-DDT18 Endrin aldehyde19 Endosulfan sulfate20 Methoxychlor21 Endrin ketone22 Decachlorobiphenyl

Detailed conditions are available on-line at wwwmn-netcomaAAs

Peaks1 Pentachlorobenzene2 246-Tribromoanisole3 Tetrachloro-14-dimethoxy-

benzene4 α-BHC5 Pentachloroanisole6 HCB7 γ-BHC8 β-BHC9 Heptachlor10 ε-BHC11 Aldrin12 1234-Tetrachloro-

naphthalene (TCN)13 PCB-10314 Oxychlordane15 cis-Heptachlor epoxide

16 24-DDE17 trans-Chlordane18 cis-Chlordane

trans-Nonachlor19 Endosulfan I20 44-DDE21 Dieldrin22 24-DDD23 Endrin24 24-DDT25 cis-Nonachlor26 44-DDD27 Endosulfan II28 44-DDT29 Parlar 4130 Parlar 4031 Parlar 4432 Endosulfan sulphate33 Parlar 5034 Mirex

1

2

3

4

5

6

7 8

9 10

11

12

1314

15

17

18

1920

21

2216

64 12108 14 min

infomn-netcom wwwmn-netcom6 7

Product information Ordering informationStep Product Pack of REFSPE 1 CHROMABONDreg HR-X 3 mL 60 mg 30 730936

CHROMABONDreg vacuum manifold for 12 columns 1 730150SPE 2 (QuEChERS) CHROMABONDreg QuEChERS Mix I (citrate extraction mix) 50 730970

CHROMABONDreg QuEChERS Mix III (Diamino clean-up mix) 50 730972SPE 3 CHROMABONDreg HR-XC 3 mL 200 mg 30 730952

CHROMABONDreg vacuum manifold for 12 columns 1 730150Filtration Disposable filters CHROMAFILreg Xtra PET-4525 100 729220

Disposable filters CHROMAFILreg Xtra PTFE-4525 100 729205Vials and caps 15 mL screw neck vials N 9 amber label and scale 100 702284

Ready assembled screw closures N 9 blue center hole with septum Silicone white PTFE red

100 7022871

HPLCColumn EC 1254 NUCLEODURreg C18 Gravity 5 μm 1 76010040Guard column EC 43 NUCLEODURreg C18 Gravity 5 μm 3 76190330Guard column holder Column Protection System 1 718966GC 1Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film 1 72642060GC 2Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film 1 72616230

Visit us at wwwmn-netcomchroma to get more helpful information

Selection tools for

Vials and caps

Syringe filters

Troubleshooting guidesGC and HPLC

Detailed product information

hellipand much more

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL

EN ISO 9001 2008CERTIFIED

Food safety made easy with products from

MACHEREY-NAGEL

Vol 8

Additives

Vol 6

Mycotoxins

Vol 2

Vitamins

Vol 4

Acrylamide

Vol 1

Melamine

Vol 5

Sugars Sweeteners

Vol 3

AntibioticsVol 7

Pesticides

KATE

N20

0123

Foc

us F

lyer

Foo

d Vo

l 7

en1

10

031

5 PD

Pr

inte

d in

Ger

man

yIm

age

cred

its copy

Tija

na o

lga

dem

schi

shin

a P

ierre

bril

lot

Pete

r Her

mes

Fur

ian

ar

enaf

otou

k fo

vito

nic

eday

rr1

45 a

irbor

ne77

Sl

y SA

DEQ

ndash fo

tolia

com

Page 5: CHROMATOGRAPH - hplc.sk · CHROMATOGRAPH Think about food Care about safety  MACHEREY-NAGEL GmbH & Co. KG · Neumann-Neander-Str. 6 8 · 52355 Düren · Deutschland  Frankreich:

infomn-netcom wwwmn-netcom4 5

Sample preparation and analysis Fungicides carbendazime and thiabendazole from fruit juiceSolid phase extraction

MN AAp MNo 304740Sample pretreatment see wwwmn-netcomaAAs

c Column type CHROMABONDreg HR-XC 3 mL 200 mg REF 730952

Column conditioning 5 mL methanol then 5 mL 2 NH3 (Do not let run the column dry)Sample aspiration The prepared sample is passed through the column by vacuumWashing impurities are removed with the following washing mixtures a) 2 mL 2 NH3 b) 2 mL 30 methanol ndash 5 NH3 c) 2 mL 01 molL HCl d) 2 mL methanolDrying with nitrogen or airElution 4 mL methanol 5 NH3

It is recommended to filter the prepared sample through dis-posable filters CHROMAFILreg Xtra PET-4525 REF 729220

HPLC analysisMN AAp MNo 122200

Column EC 1254 NUCLEODURreg C18 Gravity 5 μm REF 76010040

0 2 4 6 8 10 min

2

1

Peaks1 Carbendazime

OCH3NH

NHN

O2 ThiabendazoleNN

S NH

Detailed conditions are available online at wwwmn-netcomaAAs

MN suggests using guard columns to protect your main column and significantly increase column life

The Column Protection System (REF 718966) is suitable for all analytical HPLC columns with 116 fittings

infomn-netcom wwwmn-netcom6 7

Analysis Subsequent analysis GCPesticides from cod liver oil

MN AAp MNo 213270R Looser K Ballschmiter J Chromatogr A 836 271ndash284 (1999)Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film

REF 72642060

1

4

2

7

8

9

10

11

12

13

1415

16

1719

20

21

2223

24

2527

30

31

33

3432

29

26 2818

3 4

5

6

10 20 30 40 50min

b)

a)

It is recommended to filter the prepared sample through disposable filters CHROMAFILreg PTFE-4525 REF 729205

Organochlorine pesticides (EPA 8081)MN AAp MNo 213630

Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film REF 72616230

Peaks1 2456-Tetrachloro-

m-xylene2 α-BHC3 γ-BHC (Lindane)4 Heptachlor5 β-BHC6 Aldrin7 δ-BHC8 Heptachlor epoxide9 γ-Chlordane10 α-Chlordane11 Endosulfan I

12 44-DDE13 Dieldrin14 Endrin15 44-DDD16 Endosulfan II17 44-DDT18 Endrin aldehyde19 Endosulfan sulfate20 Methoxychlor21 Endrin ketone22 Decachlorobiphenyl

Detailed conditions are available on-line at wwwmn-netcomaAAs

Peaks1 Pentachlorobenzene2 246-Tribromoanisole3 Tetrachloro-14-dimethoxy-

benzene4 α-BHC5 Pentachloroanisole6 HCB7 γ-BHC8 β-BHC9 Heptachlor10 ε-BHC11 Aldrin12 1234-Tetrachloro-

naphthalene (TCN)13 PCB-10314 Oxychlordane15 cis-Heptachlor epoxide

16 24-DDE17 trans-Chlordane18 cis-Chlordane

trans-Nonachlor19 Endosulfan I20 44-DDE21 Dieldrin22 24-DDD23 Endrin24 24-DDT25 cis-Nonachlor26 44-DDD27 Endosulfan II28 44-DDT29 Parlar 4130 Parlar 4031 Parlar 4432 Endosulfan sulphate33 Parlar 5034 Mirex

1

2

3

4

5

6

7 8

9 10

11

12

1314

15

17

18

1920

21

2216

64 12108 14 min

infomn-netcom wwwmn-netcom6 7

Product information Ordering informationStep Product Pack of REFSPE 1 CHROMABONDreg HR-X 3 mL 60 mg 30 730936

CHROMABONDreg vacuum manifold for 12 columns 1 730150SPE 2 (QuEChERS) CHROMABONDreg QuEChERS Mix I (citrate extraction mix) 50 730970

CHROMABONDreg QuEChERS Mix III (Diamino clean-up mix) 50 730972SPE 3 CHROMABONDreg HR-XC 3 mL 200 mg 30 730952

CHROMABONDreg vacuum manifold for 12 columns 1 730150Filtration Disposable filters CHROMAFILreg Xtra PET-4525 100 729220

Disposable filters CHROMAFILreg Xtra PTFE-4525 100 729205Vials and caps 15 mL screw neck vials N 9 amber label and scale 100 702284

Ready assembled screw closures N 9 blue center hole with septum Silicone white PTFE red

100 7022871

HPLCColumn EC 1254 NUCLEODURreg C18 Gravity 5 μm 1 76010040Guard column EC 43 NUCLEODURreg C18 Gravity 5 μm 3 76190330Guard column holder Column Protection System 1 718966GC 1Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film 1 72642060GC 2Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film 1 72616230

Visit us at wwwmn-netcomchroma to get more helpful information

Selection tools for

Vials and caps

Syringe filters

Troubleshooting guidesGC and HPLC

Detailed product information

hellipand much more

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL

EN ISO 9001 2008CERTIFIED

Food safety made easy with products from

MACHEREY-NAGEL

Vol 8

Additives

Vol 6

Mycotoxins

Vol 2

Vitamins

Vol 4

Acrylamide

Vol 1

Melamine

Vol 5

Sugars Sweeteners

Vol 3

AntibioticsVol 7

Pesticides

KATE

N20

0123

Foc

us F

lyer

Foo

d Vo

l 7

en1

10

031

5 PD

Pr

inte

d in

Ger

man

yIm

age

cred

its copy

Tija

na o

lga

dem

schi

shin

a P

ierre

bril

lot

Pete

r Her

mes

Fur

ian

ar

enaf

otou

k fo

vito

nic

eday

rr1

45 a

irbor

ne77

Sl

y SA

DEQ

ndash fo

tolia

com

Page 6: CHROMATOGRAPH - hplc.sk · CHROMATOGRAPH Think about food Care about safety  MACHEREY-NAGEL GmbH & Co. KG · Neumann-Neander-Str. 6 8 · 52355 Düren · Deutschland  Frankreich:

infomn-netcom wwwmn-netcom6 7

Analysis Subsequent analysis GCPesticides from cod liver oil

MN AAp MNo 213270R Looser K Ballschmiter J Chromatogr A 836 271ndash284 (1999)Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film

REF 72642060

1

4

2

7

8

9

10

11

12

13

1415

16

1719

20

21

2223

24

2527

30

31

33

3432

29

26 2818

3 4

5

6

10 20 30 40 50min

b)

a)

It is recommended to filter the prepared sample through disposable filters CHROMAFILreg PTFE-4525 REF 729205

Organochlorine pesticides (EPA 8081)MN AAp MNo 213630

Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film REF 72616230

Peaks1 2456-Tetrachloro-

m-xylene2 α-BHC3 γ-BHC (Lindane)4 Heptachlor5 β-BHC6 Aldrin7 δ-BHC8 Heptachlor epoxide9 γ-Chlordane10 α-Chlordane11 Endosulfan I

12 44-DDE13 Dieldrin14 Endrin15 44-DDD16 Endosulfan II17 44-DDT18 Endrin aldehyde19 Endosulfan sulfate20 Methoxychlor21 Endrin ketone22 Decachlorobiphenyl

Detailed conditions are available on-line at wwwmn-netcomaAAs

Peaks1 Pentachlorobenzene2 246-Tribromoanisole3 Tetrachloro-14-dimethoxy-

benzene4 α-BHC5 Pentachloroanisole6 HCB7 γ-BHC8 β-BHC9 Heptachlor10 ε-BHC11 Aldrin12 1234-Tetrachloro-

naphthalene (TCN)13 PCB-10314 Oxychlordane15 cis-Heptachlor epoxide

16 24-DDE17 trans-Chlordane18 cis-Chlordane

trans-Nonachlor19 Endosulfan I20 44-DDE21 Dieldrin22 24-DDD23 Endrin24 24-DDT25 cis-Nonachlor26 44-DDD27 Endosulfan II28 44-DDT29 Parlar 4130 Parlar 4031 Parlar 4432 Endosulfan sulphate33 Parlar 5034 Mirex

1

2

3

4

5

6

7 8

9 10

11

12

1314

15

17

18

1920

21

2216

64 12108 14 min

infomn-netcom wwwmn-netcom6 7

Product information Ordering informationStep Product Pack of REFSPE 1 CHROMABONDreg HR-X 3 mL 60 mg 30 730936

CHROMABONDreg vacuum manifold for 12 columns 1 730150SPE 2 (QuEChERS) CHROMABONDreg QuEChERS Mix I (citrate extraction mix) 50 730970

CHROMABONDreg QuEChERS Mix III (Diamino clean-up mix) 50 730972SPE 3 CHROMABONDreg HR-XC 3 mL 200 mg 30 730952

CHROMABONDreg vacuum manifold for 12 columns 1 730150Filtration Disposable filters CHROMAFILreg Xtra PET-4525 100 729220

Disposable filters CHROMAFILreg Xtra PTFE-4525 100 729205Vials and caps 15 mL screw neck vials N 9 amber label and scale 100 702284

Ready assembled screw closures N 9 blue center hole with septum Silicone white PTFE red

100 7022871

HPLCColumn EC 1254 NUCLEODURreg C18 Gravity 5 μm 1 76010040Guard column EC 43 NUCLEODURreg C18 Gravity 5 μm 3 76190330Guard column holder Column Protection System 1 718966GC 1Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film 1 72642060GC 2Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film 1 72616230

Visit us at wwwmn-netcomchroma to get more helpful information

Selection tools for

Vials and caps

Syringe filters

Troubleshooting guidesGC and HPLC

Detailed product information

hellipand much more

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL

EN ISO 9001 2008CERTIFIED

Food safety made easy with products from

MACHEREY-NAGEL

Vol 8

Additives

Vol 6

Mycotoxins

Vol 2

Vitamins

Vol 4

Acrylamide

Vol 1

Melamine

Vol 5

Sugars Sweeteners

Vol 3

AntibioticsVol 7

Pesticides

KATE

N20

0123

Foc

us F

lyer

Foo

d Vo

l 7

en1

10

031

5 PD

Pr

inte

d in

Ger

man

yIm

age

cred

its copy

Tija

na o

lga

dem

schi

shin

a P

ierre

bril

lot

Pete

r Her

mes

Fur

ian

ar

enaf

otou

k fo

vito

nic

eday

rr1

45 a

irbor

ne77

Sl

y SA

DEQ

ndash fo

tolia

com

Page 7: CHROMATOGRAPH - hplc.sk · CHROMATOGRAPH Think about food Care about safety  MACHEREY-NAGEL GmbH & Co. KG · Neumann-Neander-Str. 6 8 · 52355 Düren · Deutschland  Frankreich:

infomn-netcom wwwmn-netcom6 7

Product information Ordering informationStep Product Pack of REFSPE 1 CHROMABONDreg HR-X 3 mL 60 mg 30 730936

CHROMABONDreg vacuum manifold for 12 columns 1 730150SPE 2 (QuEChERS) CHROMABONDreg QuEChERS Mix I (citrate extraction mix) 50 730970

CHROMABONDreg QuEChERS Mix III (Diamino clean-up mix) 50 730972SPE 3 CHROMABONDreg HR-XC 3 mL 200 mg 30 730952

CHROMABONDreg vacuum manifold for 12 columns 1 730150Filtration Disposable filters CHROMAFILreg Xtra PET-4525 100 729220

Disposable filters CHROMAFILreg Xtra PTFE-4525 100 729205Vials and caps 15 mL screw neck vials N 9 amber label and scale 100 702284

Ready assembled screw closures N 9 blue center hole with septum Silicone white PTFE red

100 7022871

HPLCColumn EC 1254 NUCLEODURreg C18 Gravity 5 μm 1 76010040Guard column EC 43 NUCLEODURreg C18 Gravity 5 μm 3 76190330Guard column holder Column Protection System 1 718966GC 1Column OPTIMAreg δ-3 60 m x 025 mm ID 025 μm film 1 72642060GC 2Column OPTIMAreg 17 MS 30 m x 025 mm ID 025 μm film 1 72616230

Visit us at wwwmn-netcomchroma to get more helpful information

Selection tools for

Vials and caps

Syringe filters

Troubleshooting guidesGC and HPLC

Detailed product information

hellipand much more

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL

EN ISO 9001 2008CERTIFIED

Food safety made easy with products from

MACHEREY-NAGEL

Vol 8

Additives

Vol 6

Mycotoxins

Vol 2

Vitamins

Vol 4

Acrylamide

Vol 1

Melamine

Vol 5

Sugars Sweeteners

Vol 3

AntibioticsVol 7

Pesticides

KATE

N20

0123

Foc

us F

lyer

Foo

d Vo

l 7

en1

10

031

5 PD

Pr

inte

d in

Ger

man

yIm

age

cred

its copy

Tija

na o

lga

dem

schi

shin

a P

ierre

bril

lot

Pete

r Her

mes

Fur

ian

ar

enaf

otou

k fo

vito

nic

eday

rr1

45 a

irbor

ne77

Sl

y SA

DEQ

ndash fo

tolia

com

Page 8: CHROMATOGRAPH - hplc.sk · CHROMATOGRAPH Think about food Care about safety  MACHEREY-NAGEL GmbH & Co. KG · Neumann-Neander-Str. 6 8 · 52355 Düren · Deutschland  Frankreich:

wwwmn-netcom

wwwmn-netcomMACHEREY-NAGEL

EN ISO 9001 2008CERTIFIED

Food safety made easy with products from

MACHEREY-NAGEL

Vol 8

Additives

Vol 6

Mycotoxins

Vol 2

Vitamins

Vol 4

Acrylamide

Vol 1

Melamine

Vol 5

Sugars Sweeteners

Vol 3

AntibioticsVol 7

Pesticides

KATE

N20

0123

Foc

us F

lyer

Foo

d Vo

l 7

en1

10

031

5 PD

Pr

inte

d in

Ger

man

yIm

age

cred

its copy

Tija

na o

lga

dem

schi

shin

a P

ierre

bril

lot

Pete

r Her

mes

Fur

ian

ar

enaf

otou

k fo

vito

nic

eday

rr1

45 a

irbor

ne77

Sl

y SA

DEQ

ndash fo

tolia

com