基质固相分散-气相色谱-离子阱串联质谱法分析牛奶中有机磷农药  

Determination of 13 organophosphorus pesticides in milk by matrix solid phase dispersion and gas chromatography-ion trap tandem mass spectrometry

作　　者：陈美瑜[1,2,3] 孙若男 林竹光[3] 

机构地区：[1]厦门大学高性能陶瓷纤维教育部重点实验室,福建省特种先进材料重点实验室 [2]厦门大学材料学院,厦门361005 [3]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,厦门361005 [4]山东检验检疫技术中心,青岛266500

出　　处：《分析试验室》2010年第9期65-69,共5页Chinese Journal of Analysis Laboratory

摘　　要：将改进的基质固相分散法与GC-MS/MS分析方法结合应用于牛奶中13种有机磷农药残留的同时分析。优化各样品前处理参数后,样品与分散剂中性氧化铝研磨后,采用乙腈超声提取。过滤浓缩后以灭线磷为内标物,采用GC-MS/MS进行定性与定量分析。从样品前处理到分析约需1 h,当样品的加标水平为50、200μg/kg时,平均加标回收率为70.4%~117.6%,相对标准偏差为0.8%~19%;除倍硫磷和毒死蜱的检测限分别为5.60和9.35μg/kg外,其它11种有机磷农药的检测限均在0.37~3.77μg/kg之间;线性范围为25~500μg/kg,相关系数均大于0.9949。A rapid method based on matrix solid phase dispersion and gas chromatography-ion trap tandem mass spectrometry was proposed for the determination of 13 organophosphorus pesticides in commercial milk.Different variables affecting MSPD procedure were studied,such as type of adsorbent,extraction solvent and solvent volume.The group of pesticides was added to milk,and then blended with deactivation neutral alumina.Pesticides were extracted from the mixture with acetonitrile in an ultrasonic bath,and then the liquor was filtered for analysis by GC-MS/MS and with ethoprophos as the internal standard.Recovery studies were performed at 50 and 200 μg/kg fortification levels for each pesticide,and the recoveries ranged from 70.4 to117.6%,while the relative standard deviations were 0.8%～19%.The detection limits of the pesticides were lower than 10 μg/kg.The linear ranges of 13 organophosphorus pesticides were 25～500 μg/kg,with correlation coefficients larger than 0.9949.The proposed method was applied to the analysis of these organophosphorus pesticides in commercial milk.

关 键 词：基质固相分散 气相色谱 离子阱串联质谱 有机磷农药 牛奶 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]