水生动物及水产品中硫丹及其代谢物残留量的气相色谱-质谱测定

建立了水生动物及水产品中农药硫丹及其代谢物残留量的气相色谱-质谱(GC-MS)测定方法;样品经溶剂提取、凝胶层析柱净化;以氦气为载气,甲烷气为反应气,程序升温及负化学源(NCI)电离方式,采用气质联用仪在选择离子监测模式下进行快速测定,保留时间和离子相对丰度比定性、外标法定量;方法定量下限为0.004 mg/kg。在鳗鱼、泥鳅、鲶鱼、虾4种样品中添加不同浓度的硫丹时,其平均添加回收率在71%~87%之间,相对标准偏差(n=10)小于10%。

Determination of Endosulfan in Aquatic Animal and in Seafood by GC -MS

A GC-MS method for the determination of endosulfan in aquatic animal and in seafood was established.Endosulfan in the targeted samples was extracted with the solvent,then cleaned up with gel chromatographic column.The carrier gas was He and reaction gas was CH4.Rapid analyses were carried out by gas chromatography-mass spectromery under NCI and selective-ion monitoring modes with programmed temperatures,qualitative analysis by the rentention times and relative intensities of selected ions and quantitation by external standard.Detection limits of this method were 0.004 mg/kg.The mean recoveries ranged from 71%-87% of fortified samples of eel,loach,catfish and shrimp,with RSD(n=10) less than 10%.