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1、第29卷第7期分析测试学报Vol129No172010年7月FENXICESHIXUEBAO(JournalofInstrumentalAnalysis)751~754蔬菜中甲胺磷等5种有机磷农药残留量的分散液-液微萃取/气质联用技术检测112222杜晓婷,周敏,张剑,曾延波,翟云云,李蕾(1.杭州市质量技术监督检测院,浙江杭州310014;2.嘉兴学院生物与化学工程学院,浙江嘉兴314001)摘要:建立了分散液-液微萃取/气相色谱质谱(DLLME/GC-MS)联用技术分析蔬菜样品中甲胺磷、甲拌磷
2、、甲基对硫磷、毒死蜱和乐果5种有机磷农药残留的新方法。优化后的萃取条件:10LL氯苯为萃取剂,110mL丙酮为分散剂,萃取时间为3min。5种有机磷农药均具有良好的线性关系,相关系数不低于01995,加标回收率为60%~95%,相对标准偏差为218%~911%,检出限为01001~01140mg/kg。应用于蔬菜中有机磷农药残留的检测,结果满意。关键词:分散液相微萃取;有机磷农药;气相色谱质谱联用;蔬菜中图分类号:O657163;F76712文献标识码:A文章编号:1004-4957(2010)0
3、7-0751-04do:i1013969/j1issn11004-4957120101071022DeterminationofFiveOrganophosphorusPesticideResiduesinVegetablesBasedonDispersiveLiquid-LiquidMicroextractionCoupledwithGasChromatography-MassSpectrometry112222DUXiao-ting,ZHOUMin,ZHANGJian,ZENGYan-bo,Z
4、HAIYun-yun,LILei(1.HangzhouInstituteofTestandCalibrationforQualityandTechnologySupervision,Hangzhou310014,China;2.SchoolofBiologicalandChemicalEngineering,JiaxingUniversity,Jiaxing314001,China)Abstrac:tAnewmethodwasdevelopedforthedeterminationof5organ
5、ophosphoruspesticideres-idues,includingmethamidophos,phorate,methylparathion,chlorpyrifos,dimethoate,invegeta-blesbydispersiveliquid-liquidmicroextraction(DLLME)coupledwithgaschromatography-massspectrometry(GC-MS).Theextractionconditionswereoptimized.
6、Agoodextractionefficiencywasobtainedbyusing10LLchlorobenzeneasextractionsolven,t018mLacetoneasdispersersolventex-tractingfor3min.Thecalibrationcurvesfor5organophosphoruspesticidesallhadgoodlinearrela-tionshipswithcorrelationcoefficientsnotlessthan0199
7、5.Thespikedrecoveriesrangedfrom60%to95%withrelativestandarddeviationsof218%-911%.Thelimitsofdetectionwereintherangeof01001-01140mg/kg.Themethodwasappliedinthedeterminationfororganophosphoruspesticideresiduesinvegetableswithsatisfactoryresults.Keywords
8、:dispersiveliquid-liquidmicroextraction(DLLME);organophosphoruspesticides;gaschromatography-massspectrometry(GC-MS);vegetables食品的基质复杂,对其中低浓度的多残留农药组分进行定性和定量分析时,通常对方法前处理的要求非常高。传统的样品前处理技术如液液萃取、索氏萃取等,普遍存在操作繁琐耗时、操作误差偏大,需要使用大量的对人体和环境有毒或有害的有机溶剂、难以实现自
