分散固相萃取-气相色谱-质谱法测定肉制品中残留的硫丹及其代谢物  

Determination of endosulfans and its metabolite in meat products by GC-MS with dispersive solid phase extraction

作　　者：曾正宏[1] 王太全[1] 王俊红[1] 丁敬香[1] 

机构地区：[1]盐城出入境检验检疫局,江苏盐城224000

出　　处：《肉类工业》2010年第6期47-50,共4页Meat Industry

摘　　要：建立了分散固相萃取-气相色谱-质谱联用法(GC-MS)检测肉制品中残留的硫丹及其代谢物。样品以乙腈为萃取溶剂,采用乙二胺-N-丙基硅烷(PSA)为吸附剂进行固相分散萃取净化,由气相色谱-质谱分时段选择离子监测技术进行测定与确证,外标法定量。方法的线性范围为0.0001～20mg/L,相关系数均在0.99以上,测定限(10S/N)均达到0.0002mg/kg,在三个浓度水平进行精密度和回收率试验,所得相对标准偏差在3.2%～6.2%之间,回收率在75%～96%之间。A gas chromatography-mass spectrometry（GC-MS）with dispersive solid phase extraction （DSPE） method was established for the simultaneous determination of endosulfans and its metabolite in meat products.The residues interested were extracted from the samples with acetonitrile.The combined extraction was concentrated to dryness and redissolved in acetonitrile,then cleaned up by dispersive solid-phase extraction with sorbents of primary secondary amine（PSA）.The residues were determined and confirmed by GC-MS in selected ion monitoring mode using external standard method.The linearity range of the method was from 0.0001mg/L to 20 mg/L（r0.99）,and quantitative detection limits （S/N=10） both reached 0.002 mg/kg.The relative standard deviations were between 3.2% and 6.2%,and the recoveries were between 75% and 96% at three concentration levels（0.001,0.005,0.01mg/kg）.

关 键 词：肉制品 硫丹 分散固相萃取 气相色谱-质谱法 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程]