鱼、虾、贝中硫丹残留量的气相色谱测定  

Determination of Endosulfan Residues in Fish,Shrimp and Shellfish by GC

作　　者：柯常亮[1] 陈洁文[1] 林钦[1] 甘居利[1] 

机构地区：[1]农业部海水养殖生态与质量控制重点开放实验室,广东省渔业生态环境重点实验室,中国水产科学研究院南海水产研究所,广州510300

出　　处：《农药》2009年第7期515-518,共4页Agrochemicals

基　　金：中国水产科学研究院重点基金项目(2003-05-04);中央级公益性科研院所基本科研业务费专项资金项目(编号2007-TS-20和2008TS07)

摘　　要：建立了鱼、虾、贝中硫丹的气相色谱测定方法。采用乙腈-乙酸乙酯混合液超声萃取,于冰箱中-18℃冷凝除脂,经无水硫酸钠、氧化铝和Florisil硅土复合柱层析净化,所得试样溶液用气相色谱法测定硫丹的残留量,外标法定量。α-硫丹、β-硫丹线性范围均为0.001～0.200mg/L,实验室得出α-硫丹、β-硫丹的相关系数分别为0.9997、0.9996;验证实验室得出α-硫丹、β-硫丹的相关系数分别为0.9997、0.9968,定量检测下限均为0.001mg/kg。当α-硫丹、β-硫丹在鱼、虾、贝试样中分别等量添加0.001、0.010、0.050mg/kg三个水平时,加标回收率变化范围为77.5%～108%,相对标准偏差变化范围为3.03%～14.7%。The determination method of endosulfan residues in fish, shrimp and shellfish was developed. The test sample were extracted ultrasonically with mixture solution of acetonitrile and ethyl acetate, condensed in refrigerator at -18 ℃ to degrease, purified through a complex column loaded with dry sodium sulfate, alumina and florisil successively, determined by gas chromatography and external standard method. The linear range of both α-endosulfan and β-endosulfan were from 0.001 to 0.200 mg/L, the correlation coefficients were respectively for this experiment： α-endosulfan was 0.999 7, β-endosulfan was 0.999 6, validating experiment： α-endosulfan was 0.999 7, β-endosulfan was 0.996 8, and the detection limit of both α-endosulfan and β-endosulfan were 0.001 mg/kg. In the validating tests, the two isomers were added equally into edible tissues of the four kind species at three levels of 0.001, 0.010 and 0.050 mg/kg, the recoveries ranged from 77.5 to 108%, RSD ranged from 3.03 to 14.7%.

关 键 词：鱼 虾 贝 硫丹 气相色谱 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]