气相色谱法测定水产品中硫丹及其代谢物残留  

Determination of Residues of Endosulfan and Its Metabolite in Aquatic Products by Gas Chromatography

作　　者：叶玫[1] 姜琳琳[1] 余颖[1] 

机构地区：[1]福建省水产研究所,福建厦门361012

出　　处：《食品科学》2013年第10期211-214,共4页Food Science

基　　金：福建省渔业项目地方标准制修订(闽海渔[2008]143号)

摘　　要：建立水产品中α-硫丹、β-硫丹、硫丹硫酸酯残留的气相色谱分析方法。样品经乙腈-乙酸乙酯(4:1,V/V)提取、冷冻除脂、石墨化碳黑-佛罗里硅土和中性氧化铝固相萃取柱串联净化,以电子捕获-气相色谱测定,外标法定量。硫丹各组分在0.001～0.2μg/mL范围内线性关系良好(r≥0.9996);当α-硫丹、β-硫丹、硫丹硫酸酯在对虾、草鱼、牡蛎和鳗鲡中的添加量为1、10、20μg/kg三个水平时,回收率在74.1%～106%之间,相对标准偏差(RSD)为1.22%～7.79%;α-硫丹、β-硫丹、硫丹硫酸酯的检出限(LOD)分别为0.035、0.06、0.06μg/kg,最低定量限(LOQ)均为1.00μg/kg。适用于鱼类、甲壳类、贝类中硫丹及其代谢物污染的监测。A gas chromatography method was established to analyze residues of α-endosulfan,β-endosulfan and endosulfan sulfate in aquatic products.Samples were extracted with acetonitrile and ethyl acetate（4：1,V/V）,frozen-degreased,purified with tandem SPE columns（carbon-florisil followed by neutral alumina）,and analyzed by gas chromatography with electron capture detector（GC-ECD） and quantified by an external standard method.Each compound showed a good linear relationship over the concentration range of 0.001–0.2 μg/mL.The recovery rates for shrimp,grass carp,oyster and eel spiked with three different levels of endosulfan at 1,10 μg/kg and 20 μg/kg ranged from 74.1% to 106%,with RSD between 1.22% and 7.79%.The limits of detection（LOD） for α-endosulfan,β-endosulfan and endosulfan sulfate were 0.035,0.06 μg/kg and 0.06 μg/kg,respectively,and the limit of quantitation（LOQ） for all of them was 1.00 μg/kg.The method can be applied in the detection of residues of endosulfan and its metabolites in fish,crustacean and shellfish.

关 键 词：α-硫丹 β-硫丹 硫丹硫酸酯 残留 气相色谱法 水产品 

分 类 号：O657.7[理学—分析化学]