两种水产品中农药多残留分析的样品前处理方法_省略_11种农药和相关

20085May2008ChineseJournalofChromatographyVo.l26No.3292~300:20080120:,.Te:l(0591)38132966,Emai:[e-mail]().111苏建峰1,林谷园2,连文浩1,张金虎1,陈冬花1(1.,350015;2.,350300):,111,(1!1!1),;∀,,,Envi18PSA(GCMS)(SIM),,GCMS,(S/N=3)0001~0026mg/kg;025mg/kg,72%~113%,(RSDs)34%~121%;∀51%~127%(70%~120%94%),RSDs32%~138%:;;;;:O658:A:10008713(2008)03029209:Twosamplepretreatmentmethodsandtheirapplicationsinthedeterminationof111pesticidesandrelatedchemicalsinaquaticproductsSUJianfeng1,LINGuyuan2,LIANWenhao1,ZHANGJinhu1,CHENDonghua1(1.FujianFairreachFoodSafetyTestingCo.,Ltd.,Fuzhou350015,China;2.FuqingEntryExitInspectionandQuarantineBureau,Fuqing350300,China)Abstract:Twosamplepretreatmentmethodsweredevelopedandappliedtodetermine111residuesofpesticidesinaquaticproducts.ForMethod,theresidueswereextractedfromhomogenizedtissuewithacetoneethylacetatenhexane(1!1!1,v/v/v),andthenwereredissolvedinacetonitrile;forMethod∀,theresidueswereextractedfromhomogenizedtissuewithacetonitrile-waterunderultrasonication,andthenwereseparatedbyliquidliquidpartition.Thesupernatantswerepurifiedusingsolidphaseextraction(Envi18andPSAcolumns)priortotheGCMSanalysis.Thedeterminationwasperformedinselectedionmonitoring(SIM)modewiththeexternalcalibrationforquantitativeanalysis.Undertheoptimalconditions,thedetectionlimits(S/N=3)forresiduesofpesticideswereintherangesof0.001-0.026mg/kg.TherecoveriesofMethodforthespikedstandardsatconcentrationof0.25mg/kgwere72%-113%withtherelativestandarddeviations(RSDs)of3.4%-12.1%.TherecoveriesofMethod∀were51%-127%,amongwhichtherecoveriesfor94%pesticideswerebetween70%and120%withtheRSDsof3.2%-13.8%.Keywords:solidphaseextraction(SPE);gaschromatographymassspectrometry(GCMS);samplepretreatment;multiresidualpesticides;aquaticproducts,,#∃,,3,:111,,,,[1-9]2003QuEChERS(quick,easy,cheap,effective,ruggedandsafe)[10],,[11,12](GPC),,,,,(SPE),111,,∀,,,(GCMS),11.16890N5975B,7683,(EI)(Agilent);:DB5MS(30m%025mm%025m);T18basic(IKA);4000r/min(SIGMA);(HEIDOLPH);DC12();(IKA);DRSIGMA;Envi18(2000mg)PSA(500mg)SUPELCO;,;1.21.2.1样品提取方法:2g(001g)50mL,(1!1!1)15mL7g,15000r/min1min,10mL,,4000r/min5min40mL;15mL,,1min,15min(2),4000r/min5min;:6mL,,4000r/min5min,3,18mL方法∀3g(001g)50mL,15mL5mL,15000r/min1min,5g,1min,15min(2),4000r/min10min,10mL,1.2.2样品净化Envi18PSA,,2cm,10mL,∀,(10mL,∀18mL),,,(1!1)1mL,GCMS1.3GC:(99999%),,10mL/min;260&;2L,;:60&(2min)20&/min120&4&/min160&2&/min170&(2min)2&/min190&(2min)3&/min230&(2min)6&/min280&(10min)MS:280&;230&;150&;(EI),70eV;400V11111∋293∋261Table1Retentiontimes,quantitativeandqualitativeionsandparametersfordeterminationofanalytesbySIMNo.t*R/minCompoundQuantitativeion(m/z)Qualitativeions(m/z)Dwelltime/msGroupGroupstarttime/min113.08propham()179120,137100111.00216.20folimat()156110,141100214.94316.90demeton()8889,171100316.61417.28diphenylamine()169167,16850417.11517.57ethoprophos()158139,200618.95monocrotophos()127192,22330518.37719.28phorate()260121,231819.38BHC()219181,183920.24dimethoate()8793,125100619.911020.87simazine()201173,18620720.591120.95BHC()219181,1831221.07PCNB()237249,2951321.24atrazine()200173,2151421.49!BHC(!)219181,1831522.14terbufos()231153,288100821.861622.90pyrimethanil()198199,20050922.571722.92diazinon()179137,3041823.70∀BHC(∀)219181,183201023.371924.02triallate()268143,2702024.11etrimfos()292181,2772124.26tefluthrin()177161,1972224.70pirimicarb()166138,2381001124.492326.11PCB28()256186,258301225.532426.17chlorpyrifosmethyl()286125,2882526.21acetochior()146162,2232626.64vinclozolin()285198,212201326.452726.69parathionmethyl()263109,1252826.88alachlor()160188,2372927.01heptachlor()272237,3373027.60metalaxyl()206234,2491001427.343128.01prometryn()241184,226501527.783228.11S2()13079,1323328.89fenitrothion()277125,260201628.563428.96PCB52()292220,2553528.97pirimiphosmethyl()290276,3053628.98terbutryn()226170,2413729.83aldrin()263265,293151729.483830.05malathion()173143,1583930.26chlorpyrifos()199258,3144030.30thiobencarb()100125,2574130.64fenthion()278153,1694230.94parathion()291186,2354331.23trazodone()208181,210501831.044431.29isocarbophos()136230,2894532.12fosthiazate()195126,2831001931.7832.34fosthiazate∀(∀)195126,2834633.09pendimethalin()252162,281502032.724733.26heptachlorepoxide()35381,3554833.59penconazole()159161,2481002133.394934.01fipronil()367351,369502233.775034.25isofenphos()213185,2555134.70quinalphos()146157,298152334.485234.86procymidone()28396,2855335.14allethrin()123107,13635.24allethrin∀(∀)123107,1365435.52chlordane()373272,375∋294∋3,:1111()Table1(Continued)No.t*R/minCompoundQuantitativeion(m/z)Qualitativeions(m/z)Dwelltime/msGroupGroupstarttime/min5535.74methidathion()14585,3025636.49paclobutrazol()236167,238152436.175736.52PCB101()326254,2915836.57endosulfan()241265,3395936.64tetrachlorvinphose()331109,3296036.67!chlordane(!)373272,3756137.88chlorfluazuron()321323,3561002537.376238.28fenamiphos()303154,288152638.076338.48prothiofos()309162,2676438.60flutolanil()173145,3236538.80isoprothiolane()189231,2906638.81preti