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20097July2009ChineseJournalofChromatographyVo.l27No.4391~400*:,.Emai:lswj9722418@yahoo.com.cn.:(No.200810099,200810219)(No.20575027)(No.2006BAK02A08).:20090218107沈伟健1*,余可垚1,桂茜雯1,蒋原1,赵增运1,沈崇钰1,吴斌1,储晓刚2(1.,210001;2.,100025):(QuEChERSGCMS/MS)1071%,,005~1mg/L;(LOQ)10g/kg;10g/kg,460%~130%,(RSD)153%107,:;;;;:O658:A:10008713(2009)04039110:Determinationof107pesticideresiduesinvegetablesusingofflinedispersivesolidphaseextractionandgaschromatographytandemmassspectrometrySHENWeijian1*,YUKeyao1,GUIQianwen1,JIANGYuan1,ZHAOZengyun1,SHENChongyu1,WUBin1,CHUXiaogang2(1.FoodLaboratoryofJiangsuEntryExitInspectionandQuarantineBureau,Nanjing210001,China;2.ChineseAcademyofInspectionandQuarantine,Beijing100025,China)Abstract:Ascreeningmethodwasdevelopedforthedeterminationof107pesticideresiduesinvegetablesusingofflinedispersivesolidphaseextraction(DSPE)andgaschromatographytandemmassspectrometry(GCMS/MS).Thepesticidesinterestedwereextractedfromthesampleswithacetonitrile(saturatedbynhexane)containing1%aceticacidandsimultaneouslyseparatedbyliquidliquidpartitioningwithaddinganhydrousmagnesiumsulfateplussodiumacetatefollowingbyasimplecleanupstepknownasdispersivesolidphaseextraction.TheextractsweredeterminedbyGCMS/MSusingexternalstandardmethod.Themethodwasreliableandstablethattherecoveriesofalmostallpesticideswereintherangefrom60%to130%atthespikedlevelof10g/kgintofourvegetablematrixes(garlic,greenbean,radishandspinach)andtherelativestandarddeviations(RSDs)wereallnotmorethan153%.Thelinearityofthemethodwasgoodbetween005mg/Land1mg/L,andalllimitsofquantification(LOQs)lessthan10g/kg.Themethodisselectivewithnointerference,especiallyinthecomplicatedgarlicmatrix.Keywords:gaschromatographytandemmassspectrometry(GCMS/MS);selectedreactionmonitoring(SRM);dispersivesolidphaseextraction(DSPE);multiplepesticideresidues;vegetables27,,,,,(GC)[1](GCMS)[2,3](LCMS/MS)[4]GC,,;GCMS,;LCMS/MS,,,GCMS/MS107,GCMS(),,,2003Steven,QuEChERS(Quick,Easy,Cheap,Effective,RuggedandSafe)[5-9]QuEChERS(),;,,QuEChERS,,11.1Varian3800GC320MS(),BuCHIR200(BCHI),SHZ88()1.2,1%()PestiCard(120~400)N(PSA)(40~60)C18(40~60)SepaxUCT107(1)(!980%)Dr.Ehrenstorfer1.3:10mg(001mg),10mL,,1g/L,4∀:01mL25mL,,4mg/L1000,500,200,10050g/L,4∀1.410g(001g),250mL,20mL,15g6g,40min150mL20mL,40∀2mL,200mgPSAC18,1min,,045m,GCMS/MS1.5GCMS/MS1.5.1GC条件VF5ms(30m#025mm#025m);,50∀(2min),30∀/min180∀,5∀/min300∀(5min)(!99999%);10mL/min;300∀;280∀;1L,,1min1.5.2MS/MS条件:230∀;:40∀;:(EI),:70eV;:450min;:(!99999%);Q1:300,Q2:100;:(SRM)122.1[5-7]QuEChERS,,;∃392∃4,:107,;PSA;C18,,,[5-7]QuEChERS31107Table1Retentiontimewindows,retentiontimes,EIMS/MSconditions,linearequationsandcorrelationcoefficientsforthedeterminationof107pesticidesNo.PesticideRetentiontimewindow/mintR/minPrecursorion%Production(m/z)Collisionenergy/eVLinearequation**r21mevinphos4.60-13.177.66127%109*-10y=180x+430.9998()192%127-102propham7.95179%137*-6y=8531x-423071.0000()179%93-123molinate8.71126%55*-10y=17357x-4043000.9922()187%126-54tecnazene9.19213%142*-20y=1386.6x-130270.9960()213%178-105ethalfluralin9.48316%276*-10y=993x-84170.9973()292%264-106diphenylamine9.53169%139*-35y=4014x-764581.0000()169%77-357trifluralin9.62306%264*-10y=7323x-505920.9994()264%206-108benfluralin9.67292%206*-10y=964x-104250.9969()292%160-209chlorpropham9.70213%127*-15y=2023x-256100.9988()213%171-510dioxabenzofos9.88216%201*-10y=24518x-311380.9989()216%137-2011cadusafos9.99159%97*-15y=3124x-249720.9948()159%131-61266610.34181%145*-15y=8448x-756500.9994()217%181-1013atrazine10.76200%104*-15y=697x-71380.9755()215%200-614dichloran10.82206%176*-10y=909x-259160.9766()176%148-1015clomazone10.87125%89*-15y=6975x-766660.9962()204%107-15(1)1kg/L;,,,5kg/L,,5(2),,,(3),,,(50~250mg),;C18(100~200mg),,2.21350~1000g/L15GCMS/MS,yx(g/L),,11,50~1000g/L1071∃393∃271()Table1(Continued)No.PesticideRetentiontimewindow/mintR/minPrecursorion%Production(m/z)Collisionenergy/eVLinearequation**r21666610.94181%145*-15y=2493x-238590.9981()217%181-1017terbufos11.04231%129*-22y=8780x-842570.9950()231%175-1018!66611.11181%145*-15y=7163x-517310.9995(!)217%181-1019propyzamide11.18173%145*-13y=15749x-1547500.9989()173%109-2520fonofos11.25246%109*-20y=16376x-1438000.9994()246%137-1021isazofos()11.46161%119*-10y=13502x-311910.999222terbacil11.63161%144*-10y=2080x-206761.0000()161%88-2023∀66611.84181%145*-15y=2382x-249950.9967(∀)217%181-1024benoxacor12.06120%65*-20y=2997x-199321.0000()120%93-1525dichlofenthion12.30251%223*-10y=6391x-732520.9992()279%251-1026vinclozolin12.59285%212*-10y=1634x-142630.9975()285%198-3027tolclofosmethyl12.72265%93*-20y=3907x-387020.9957()265%220-2028ametryn12.88227%185*-6y=4155x-443810.9995()212%94-2029dithiopyr12.91354%306*-7y=11898x-246190.9969()306%286-830prometryn12.92241%184*-10y=4154x-276530.9988()241%199-1031fenchlorphos12.99285%270*-10y=2248x-261570.9956()285%93-3032terbutryn13.17-16.2513.31185%170*-6y=9994x-746070.9986()241%185-533thiazopy13.59327%277*-30y=613x-18700.9991()327%306-634chlorpyrifos13.81314%258*-15y=3343x-360380.9994()314%286-1035chlorthaldimethyl13.99332%301*-10y=5322x-431020