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1、气相色谱-负离子化学源-质谱法分析牛奶饮品和奶粉中多种有机磷农药残留1*11111,211林竹光陈美瑜张莉莉孙若男马玉涂逢樟李小波陈招斌(1.厦门大学化学化工学院化学系，现代分析科学教育部重点实验室，福建厦门361005；2.龙岩学院化学与材料工程系，福建龙岩364000)摘要将气相色谱-负离子化学源-质谱法(GC-NCI-MS)应用于牛奶饮品和奶粉中19种有机磷农药残留的同时分析。牛奶饮品和奶粉经乙腈提取剂超声提取、Florisil硅藻土和中性氧化铝双净化剂同时净化及正己烷/乙酸乙酯(1/1，v/v)混合洗脱剂洗脱后，以三苯基磷酸
2、酯为内标物，采用GC-NCI-MS的选择离子监测方式(SIM)定性与定量分析。当牛奶饮品和奶粉的加标浓度水平为20、100、500µg/kg时，平均加标回收率为64.5%~129%，相对标准偏差为2%~20%；除喹硫磷的方法检测限(MDL)为2.4µg/kg外，其余18种有机磷农药的MDL均小于1.0µg/kg；线性范围为10~500µg/kg，相关系数均大于0.9988，此分析方法成功地应用于牛奶饮品和奶粉中多种痕量有机磷农药残留的分析。关键词气相色谱；负化学离子源；质谱；牛奶饮品；奶粉；有机磷农药；农药残留Multiresidu
3、edeterminationof19organophosphorouspesticidesinmilkdrinkandmilkpowderbygaschromatography-negativechemicalionization-massspectrometry1*11111,21LinZhuguang,ChenMeiyu,ZhangLili,SunRuonan,MaYu,TuFengzhang,LiXiaobo,Chen1Zhaobin(1.DepartmentofChemistryandTheKeyLaboratoryofAn
4、alyticalSciencesoftheMinistryofEducation,CollegeofChemistryandChemicalEngineering,XiamenUniversity,Xiamen361005,China.2.DepartmentofChemistryandMaterialEngineering,LongyanCollege,Longyan,364000,China.)AbstractArapidmethodwasdevelopedforthedeterminationof19organophospho
5、rouspesticidesincommercialmilkdrinkandmilkpowder.Aftertheoptimizationofdifferentparameterssuchastheextractionsolvent,pesticideswereextractedfrommilkdrinkormilkpowderwithacetonitrileinanultrasonicbathandcleaneduponaFlorisilandneutralaluminacolumn,thenweredeterminedbygas
6、chromatographywithnegativechemicalionizationmassspectrometricdetectionintheselectedionmonitoringmode,andwithtriphenylphosphateasinternalstandard.Recoverystudieswereperformedat20,100and500µg/kgfortificationlevelsforeachpesticide,andtherecoveriesrangedfrom64.5%to129%with
7、arelativestandarddeviationbetween2%and20%forthedifferentpesticides.Thedetectionlimitofthemethodwaslessthan1.0µg/kgformostofpesticidesexceptforthequinolphos.Thedevelopedmethodwaslinearovertherangeassayed10-500µg/kgwithdeterminationcoefficients>0.9988.Theproposedmethodwa
8、ssuccessfullyappliedtotheanalysisofthesecompoundsinmilkdrinkandmilkpowder.Keywordsgaschromatography(GC);negativechemi
