工作简报分散固相萃取分离气相色谱法测定银鱼中拟除虫菊酯类农药残留量曹军1,陈勇1,杨瑞章1,徐邦兴1,王太全1,黄月芳2(1.盐城出入境检验检疫局,盐城224002;2.南通市水产品检测中心,南通226006摘要:以冰乙酸乙腈溶液为萃取溶剂,采用乙二胺N丙基硅烷(PSA、C18和石墨化炭黑固相材料分散净化技术,以气相色谱电子捕获检测器测定银鱼中6种拟除虫菊酯类农药(联苯菊酯、甲氰菊酯、高效氯氟氰菊酯、氯氰菊酯、氰戊菊酯和溴氰菊酯。该方法在0.05~1.0mgL-1范围内呈线性关系。方法的检出限(3S/N:氯氰菊酯为0.02mgkg-1,其余5种拟除虫菊酯均为0.01mgkg-1。以银鱼试样为基体,加入两种不同浓度的6种拟除虫菊酯标准溶液作回收试验,测得回收率在82.9%~106.1%之间,相对标准偏差(n=6在2.9%~7.1%之间。关键词:气相色谱法;分散固相萃取;拟除虫菊酯类农药;银鱼中图分类号:O657.7文献标志码:A文章编号:10014020(201010117603GCDeterminationofResidualAmountofPyrethroidPesticidesinWhitebaitwithSeparationbyDispersiveSolidPhaseExtractionCAOJun1,CHENYong1,YANGRuizhang1,XUBangxing1,WANGTaiquan1,HUANGYuefang2(1.YanchengEntryExitInspectionandQuarantineBureau,Yancheng224002,China;2.NantongMunicipalFisheryProductQualityTestingCenter,Nantong226006,ChinaAbstract:Sixpyrethroidpesticides,namelybifenthrin,fenpropathrin,cyhalothrin,cypermethrin,fenvalerateanddeltamethrin,inwhitebaitweredeterminedsimultaneouslybyGCwithECDafterseparationbydispersivesolidphaseextraction(DSPE.Sampleofwhitebaitwasextractedhomogeneouslywithglacialaceticacidacetonitrilesolutionasdispersionagent.TheextractobtainedwaspurifiedbyDSPEthroughcycleshakingwithethylenediamineNpropylsilane(PSA,C18andgraphitizedcarbonblack.ThesupernatantwasusedforGCECDanalysis.Linearityrangesfoundwereinthesamerangeof0.05-1.0mgL-1forthe6pyrethroidpesticides.Detectionlimits(3S/Nofthemethodobtainedwere0.01mgkg-1forcypermethrinand0.02mgkg-1fortheother5pyrethroidpesticides.Testsforrecoveryandprecisionweremadebyadditionofstandardsolutionsofthe6pyrethroidpesticideswith2differentconcentrationstowhitebaitsamplewhichwasthenanalyzedbytheproposedmethod.Valuesofrecoveryobtainedwereintherangeof82.9%-106.1%andvaluesofRSDs(n=6wereintherangeof2.9%-7.1%.Keywords:Gaschromatography;Dispersivesolidphaseextraction;Pyrethroidpesticides;Whitebait拟除虫菊酯类农药具有选择性毒性、环境中残留较少等特点,但其对哺乳动物的生殖、免疫等系统具有毒副作用[12],因此,氟氯氰菊酯、氟氰戊菊酯等收稿日期:20090711基金项目:江苏出入境检验检疫局科研计划(2009KJ33作者简介:曹军(1982-,男,安徽怀宁人,工程师,主要从事食品检验检疫。在渔业生产中已被禁用[3]。欧盟EC2162/2001规定了水产品中氯氰菊酯的残留限量为50gkg-1,溴氰菊酯为10gkg-1。日本肯定列表制度中规定了鲑形目等中氯氰菊酯、溴氰菊酯的残留限量为30gkg-1,其他的鱼及水生动物均为10gkg-1[4]。农业部公告第235号规定动物性食品中氰戊菊酯的残留限量为20~1000gkg-1,鱼肌肉中溴氰菊酯为30~500gkg-1。QuEChERS(Quick,Easy,Cheap,Effective,RuggedandSafe方法是StevenJ.Lehotay和MichelangeloAnastassiadas等提出的一种快速、简单、低成本的样品处理方法,该方法的关键是采用分散固相萃取(DSPE净化法[5],已有200余种农药等污染物残留可用该方法进行分析[613]。但将QuEChERS方法应用于水产品中拟除虫菊酯类农药多残留的分析尚未见报道。本工作以银鱼为分析对象,对QuEChERS方法进行了改进,用气相色谱法测定银鱼中拟除虫菊脂类农药残留量,为科学控制该类农药使用及进出口水产品残留农药监控提供科学依据。1试验部分1.1仪器与试剂Agilent6890气相色谱仪,配电子捕获检测器(ECD;Laborota4001型旋转浓缩仪。甲氰菊酯、联苯菊酯、高效氯氟氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯标准溶液均为100.0mgL-1。乙腈为色谱纯,正己烷、冰乙酸...