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Multi-Residue Pesticide Screening Method Using GC/MS Sky Countryman and Kory Kelly Phenomenex, Inc., Torrance, CA, USA

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Multi-Residue Pesticide Screening Method Using GC/MS Sky Countryman and Kory Kelly Phenomenex, Inc., Torrance, CA, USA GC TN-2021 Multi-Residue Pesticide Screening Method using GC/MS Sky Countryman and Kory Kelly Phenomenex, Inc., Torrance, CA, USA Pesticides are widely used by farmers to control pests, weeds be used for screening, Mass Spectrometer (MS) detection must and molds that would otherwise decrease crop production. be employed to provide positive confirmation. While this has significantly increased worldwide food ™ productions, these same pesticides pose significant health and Zebron MultiResidue columns represent a solution for all environmental risks. classes of pesticides analysis. The columns were developed using two new stationary phases that are unlike any commercially The restrictions for specific pesticides differ from one country available today. Each phase was optimized to resolve a different to the next. As world trade increases, the potential threat to set of analytes. However, both are good for a wide variety of other countries’ populations increases. This is especially true pesticides. in the European Union, where produce can be transported from one country to another quite easily. ZebronMultiResidue columns are well suited for use on all types of detectors. Both columns are MS certified, so they can also For this reason, pesticides are the subjects of increasing be used with GC/MS for multi-residue pesticide methods. The regulation. Since many different types of pesticides can be used unique selectivity offered by each phase allows for increased on the same food product, Multi-Residue screening approaches resolution of critical compounds vs. standard 5ms type phases. are used to look for more than 300 compounds at a time. Gas Retention time data is available for over 300 different pesticides Chromatography (GC) is still the most commonly used method on GC/MS, further simplifying new method development. for the majority of the pesticide classes. While ECD or NPD may 16183 23 65 Column: Zebron MultiResidue-2 11 12 15 20 24 33 42-44 56,57 79-81 87 Dimensions: 30 meter x 0.25 mm x 40 64 0.20 µm Part No.: 7HG-G017-10 Injection: Splitless at 260 °C, 1 µL 35- 68, Carrier Gas: Helium @ 0.9 mL/min 41 69 90 32 37 78 63 70 (Constant Flow) 16 38-39 73 77 Oven Program: 80 °C for 0.5 min to 150 °C @ 88 19 25 51,52 71 50 58 72 10 °C/min to 240 °C @ 4 °C/ 7 27 66, 67 47-49 83,84 min to 320 °C @ 15 °C/min 45 21, 59 75 for 3 min 55 22 46 62 86 89 13 28 76 Detector: MSD @ 320 °C; 45-400 amu 26 60, 74 82 8 30 54 61 6 17 91 34 9 29 31 53 10 14 18 85 10 12 14 16 18 min 20 22 24 min 94 98 4 107 110 106 100 109 95 92 102 99 101 104 105 103 93 96, 108 111, 97 16183 5 112 113 2 ID: 3 114 1 26 28 30 32 min App 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 min www.phenomenex.com Phenomenex products are available worldwide. For the distributor in your country, contact Phenomenex USA, International Department by telephone, fax or email: [email protected]. Australia Austria Canada Denmark France Germany tel.: 02-9428-6444 01-319-1301 (800) 543-3681 4824 8048 01 30 09 21 10 06021-58830-0 fax: 02-9428-6445 01-319-1300 (310) 328-7768 4810 6265 01 30 09 21 11 06021-58830-11 email: info@ anfrage@ info@ dkinfo@ franceinfo@ anfrage@ phenomenex.com.au phenomenex.com phenomenex.com phenomenex.com phenomenex.com phenomenex.com Ireland Italy New Zealand Puerto Rico United Kingdom USA tel.: 01 247 5405 051 736176 09-4780951 (800) 541-HPLC 01625-501367 (310) 212-0555 fax: +44 1625-501796 051 735302 09-4780952 (310) 328-7768 01625-501796 (310) 328-7768 email: eireinfo@ italiainfo@ info@ info@ ukinfo@ info@ phenomenex.com phenomenex.com phenomenex.co.nz phenomenex.com phenomenex.com phenomenex.com GC TN-2021 16184 65 79,82 Column: Zebron MultiResidue-1 87 24 20 23 33,35 41,44,45 Dimensions: 30 meter x 0.25 mm x 0.25 µm Part No.: 7HG-G016-11 42,47 Injection: Splitless at 260 °C, 1 µL Carrier Gas: Helium @ 0.9 mL/min 69,64,67 40 (Constant Flow) 71,74,78,75 Oven Program: 80 °C for 0.5 min to 150 °C @ 10 °C/min to 240 °C @ 4 °C/ min to 320 °C @ 15 °C/min 63 for 3 min 70 77 73 Detector: MSD @ 320 °C; 45-400 amu 88 32 80,76 19 25 46,48 86 39 84 36 50 27 59 15 62 66 81 89 51 12-14 60 49 4 22 52 61 68 72 28 56 30 21 94,95 26 31 37 43 83 18 53 22 24 29 11 34 96 14 16 18 min 100 107 90 110 102 106 8,5 7 58 109 92 99 105 55 112,113 2 3 104 101 114 1 6 57 93 96, 111 54 108 16 17 91 97 103 9 10 16184 ID: 8 10 12 14 16 18 20 22 24 26 28 30 32 34 min App Peak Sample Analyte Peak Sample Analyte Peak Sample Analyte Peak Sample Analyte No. No. No. No. 1 Dichlorvos 30 Phorate 60 Chlorpyrifos methyl 91 Crotoxyphos 2 EPTC 31 Dicrotophos 61 Phosphamidon 92 Stirofos 3 Butylate 32 Pentachlorophenol 62 Ronnel 93 Tokuthion 4 3,5-Dichlorobenzoic acid (methyl ester) 63 Prometryn (methyl ester) 33 Profluralin 64 Ametryn 94 Oxadiazon 5 Vernolate 34 Demeton Isomer 65 Bentazon (methyl ester) 95 Merphos Oxide 6 Pebulate 35 Prometon 66 Aspon 96 Napropamide 7 Mevinphos 36 Atraton 67 Simetryn 97 Fenamiphos 8 4-Nitrophenol 37 Monocrotophos 68 Metribuzin 98 Oxyflurofen (methyl ester) 38 Atraton Isomer 69 Methyl parathion 99 Acifluorfen 9 Mevinphos Isomer 39 Silvex (methyl ester) 70 Terbutryn 10 Trichlorfon 40 Terbufos 71 Metolachlor 100 Carboxin 11 Dicamba (methyl ester) 41 Propazine 72 Malathion 101 Ethion 12 MCPP (methyl ester) 42 Diazinon 73 DCPA 102 Tricyclazole 13 Molinate 43 Pronamide 74 Fenitrothion 103 Fensulfothion 14 Tebuthiuron 44 Atrazine 75 Chlorpyrifos 104 Carbofenotion 15 MCPA (methyl ester) 45 Simazine 76 Trichloronate 105 Famfur 16 DEET 46 Terbuthylazine 77 Triadimeton 17 Tetraethyl 47 Dioxathion 78 Pichloram (methyl) 106 Norflurazon pyrophosphate 48 Fonofos 107 Hexazinone (methyl ester) 79 Isopropalin 49 Dimethoate 108 EPN 18 Demeton 80 Fenthion 50 2,4,5-T Methyl ester 81 MGK-264 Isomer 109 Phosmet 19 Dichloroprop 51 Disulfoton (methyl ester) 82 Parathion 110 Leptophos 52 Chloramben 83 Merphos 20 Trifluralin 111 Azinphos-Methyl (methyl ester) 84 Bromacil 21 Thionazin 53 Phosphamidon Isomer 112 Fenarimol 22 Cycloate 85 Clofenvinfos Isomer 54 Secbumeton 86 MGK-624 113 Azinphos-ethyl 23 Benefin 55 Dichlofenthion 24 Propachlor 87 Pendimethalin 114 Coumaphos 56 2,4-DB (methyl ester) 88 Diphenamid 25 Ethoprop 57 Terbacil 26 Chlorpropham 89 Clofenvinfos 58 Dinoseb (methyl ester) 90 Butachlor 27 2,4-D (methyl ester) 59 Alachlor 28 Sulfotep 29 Naled For a digital copy of this Technical Note, please visit www.Phenomenex.com/TechNotes/2021 ;FCSPOBOE.VMUJ3FTJEVFBSFUSBEFNBSLTPG1IFOPNFOFY*OD1IFOPNFOFYJTBSFHJTUFSFEUSBEFNBSLPG1IFOPNFOFY*ODª1IFOPNFOFY *OD"MMSJHIUTSFTFSWFE $PQZJOHPSSFVTFPGUIJTJOGPSNBUJPOJTOPUBMMPXFEXJUIPVUXSJUUFOQFSNJTTJPOTGSPN1IFOPNFOFY GC TN-2021 Retention times for additional pesticides using Zebron MultiResidue-1 Retention Time Compound Retention Time Compound Column: Zebron MultiResidue-1 18.82 Trifluralin 24.83 Ethiofencarb Dimensions: 30 meter x 0.25 mm x 18.86 Diphenylamine 24.84 Dimethachlor 0.25 µm 18.99 Benfluralin 24.98 delta-BHC Part No.: 7HG-G016-11 Injection: Splitless at 280 °C, 1 µL 19.27 Chlordimeform 25.08 Desmetryn Carrier Gas: Constant Flow Helium 19.50 CIPC 25.23 Heptachlor 1.2 mL/min 19.57 2,3,5-Trimethacarb 25.29 Vinclozolin Oven Program: 60 °C (Hold 1 min) to 130 °C 19.63 Tebutam 25.51 Dioxacarb - C H NO at 10 °C/min to 230 °C at 2 3 4 °C/min to 300 °C 19.67 Diallate-1 25.55 Chlorothalonil (Hold @ 300 ˚C for 10 min) 19.83 Penmediapham (frag-2) 25.59 a-Spiroxamine Detector: MSD; 300 °C 20.11 Bendiocarb - C2H3NO 25.66 Propanil 20.16 MBTZ 25.73 Cymiazole 20.19 Diallate-2 25.91 Metalaxyl Retention Time Compound 20.31 Promecarb 25.94 Prometryn 6.34 Metaldehyde 20.36 Alpha-BHC 25.98 Metribuzen 7.14 Phenmedipham (frag-1) 20.55 2,6-DIPN 25.98 Ametryn 7.81 Monolinuron IP (frag) 20.66 Hexachlorobenzene 25.98 Simetryn 8.28 Propoxur - C2H3NO 21.30 Ethoxyquin 26.20 Kresoxim-Methyl 8.61 Ethiolate 21.56 Prometon 26.35 Carbaryl - C2H3NO 9.07 Isoproturon (frag) 21.58 Profluralin 26.37 3-OH Carbofuran 10.21 Bendiocarb - C2H3NO 21.65 3,4,5-Trimethacarb 26.55 Terbutryn 10.70 Carbofuran - C2H3NO 21.68 Bufencarb-1 26.57 Fuberidazole 10.85 Linuron IP (frag) 21.77 Desmedipham 26.70 Pentachlorothioanisole 11.43 EPTC/Eptam 21.79 Dichloran 26.84 Aldrin 11.85 Dichlobenil 21.86 Command/Clomazone 26.86 Ethofumesate 12.52 Biphenyl 21.97 Carbofuran 26.95 Fenpropimorph 12.78 Butylate 21.98 Simazine 26.95 Dichlofluanid 13.36 Vernolate 22.01 Monolinuron 27.04 Metolachlor 13.49 Dioxacarb - C2H3NO 22.02 Atrazine 27.05 Methiocarb 13.73 Pebulate 22.02 Terbumeton 27.14 Dursban 13.88 Etridiazole 22.23 Quintozene 27.15 Norea 14.00 3,4-Dichloroaniline 22.38 gamma-BHC (Lindane) 27.25 Dacthal/DCPA 14.36 Propham 22.45 Cycluron 27.49 Naphthalene Acetamide 14.68 Metolcarb 22.46 Terbuthylazine 27.66 Butralin 14.96 d10-Acena-phthalene 22.47 Aminocarb 27.74 Diethofencarb 15.30 Folpet IP (frag) 22.63 Fluchloralin 27.97 Triadimefon 15.44 Chloroneb 22.74 Pronamide 28.09 Isopropalin 15.71 Pentachlorobenzene 22.76 Tefluthrin 28.10 Nitrothal isopropyl 15.91 o-Phenylphenol 22.84 Isocarbamid 28.28 MGK-264 (peak-1) 15.92 Captan IP frag (THPI) 22.98 Triallate 28.39 Methfuroxan 15.95 Carbaryl - C2H3NO 23.11 Dinitramine 28.44 Tetraconazole 16.14 Molinate 23.19 Pyrimethanil 28.50 p,p’-Dicofol (frag) 16.24 Tebuthiuron 23.19 Pentachlorobenzonitrile 28.51 Cyanazine 16.38 Isoprocarb 23.25 Bufencarb-2 28.81 Pendimethalin 17.80 Tecnazene 23.58 Secbumeton Continued on next page 18.08 Fenobucarb 23.59 Mexacarbate 18.14 Propachlor 23.93 Pirimacarb 18.31 Cycloate/Ro-Neet 23.99 beta-BHC 18.40 Propoxur - C2H3NO 23.99 Fenfuram 18.50 Ethafluralin 24.19 Octhilinone 18.53 2,3,5,6-Tetrachloroaniline 24.22 beta-Spiroxamine 24.48 Pentachloroaniline For a digital copy of this Technical Note, please visit www.Phenomenex.com/TechNotes/2021 3 Zebron and MultiResidue are trademarks of Phenomenex Inc.
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