QuEChERS/GC-MS法测定水产品中的硫丹及其代谢物  

Determination of endosulfan and its metabolite in aquatic products by QuEChERS/GC-MS method

作　　者：范广宇[1] 唐秀[1] 孟祥龙[1] 姚燕林[1] 王雪婷[1] 王海涛[1] 徐文科[1] 周毅[1] 段宏安[1] 

机构地区：[1]连云港出入境检验检疫局,连云港222042

出　　处：《分析试验室》2014年第11期1301-1304,共4页Chinese Journal of Analysis Laboratory

基　　金：质检公益科技项目(201110037)资助

摘　　要：建立了QuEChERS法提取净化、气相色谱质谱联用仪测定水产品中的硫丹（α-硫丹和β-硫丹）及其代谢物硫丹硫酸盐的方法。样品用10mL乙腈提取,取1mL加入PSA和C18粉末振荡后离心,上清液过滤膜后用气相色谱质谱联用仪测定。3种物质在0.5-100μg/L范围内线性良好,在1,5,10μg/kg3个浓度水平下3种目标物平均添加回收率在72.3%-101.6%之间,RSD小于10%,定量限为0.5μg/kg,满足进出口检测要求,已应用于水产品中硫丹残留的测定。A quick, easy, cheap, effective, rugged and safe （QuEChERS） method for the determination of endosulfan（α, β ） and its metabolite endosulfan sulfate in aquatic products with gas chromatography mass sepectrometry（GC-MS） was established. Endosulfans in samples were extracted with 10 mL of acetonitrile, and then 1 mL of the supematant was transferred to a tube with addition of primary secondary amine （PSA） and C18 powder and vortex-mixed. After centrifuged, the supematant was filtered through 0. 22 μm syringe filter to the sample vial for analysis on GC-MS. The calibration curves showed good linearity in 0. 5 - 100 μg/L for each endosulfan. The mean recoveries of the endosulfans varied from 72.3% to 101.6% at the spiked levels of 1, 5, 10 μg/kg, and the relative standard deviations were less than 10%. The limit was 0.5 μg/kg. The established QuEChERS method was applied to determination of endosulfans in real samples successfully. This method can be used for the determination of endosulfans and its metabolite in aquatic products of import and export trade.

关 键 词：QuEChERS法 水产品 硫丹 气相色谱质谱联用仪 

分 类 号：O657.63[理学—分析化学]