凝胶渗透色谱净化-气相色谱法测定水产品中毒杀芬残留量  

Determination of toxaphene residues in aquatic products by gel permeation chromatography and gas chromatography

作　　者：刘慧慧[1,2] 徐英江[1,2] 邓旭修 张华威 刘云[4] 宫向红[1,2] 

机构地区：[1]山东省海洋水产研究所,烟台264006 [2]山东省海洋生态修复重点实验室,烟台264006 [3]烟台山水海产有限公司,烟台264006 [4]上海海洋大学,上海201306

出　　处：《中国渔业质量与标准》2013年第3期73-77,共5页Chinese Fishery Quality and Standards

基　　金：山东省现代农业产业技术体系刺参产业创新团队项目;国家海洋公益性行业科研专项(201105013);山东省科学技术发展计划项目(2012GHY11517);烟台市科技发展计划项目(2012134)

摘　　要：建立了水产品中毒杀芬残留量的凝胶渗透色谱净化-气相色谱检测方法。水产样品经匀浆后，用丙酮提取，经正己烷液液萃取、凝胶渗透色谱和浓硫酸净化后，用HP-5ms毛细管柱分离，电子捕获检测器检测，外标法定量。结果表明，毒杀芬在20～500μg／L浓度范围内线性良好，相关系数月≥0．998。方法检出限1．0μg／kg，在添加量2．0～20．0μgkg范围内，回收率在73．7％-78．7％之间，相对标准偏差≤6．3％。该方法灵敏、准确，可以满足水产品中毒杀芬检测要求。A new method containing gel permeation chromatography （GPC） and gas chromatography with electron - capture detection （ GC - ECD） for the determination of toxaphene in aquatic products has been developed. After hom- ogenization, the samples were extracted by acetone, and then purified by liquid - liquid extraction. A further purifica- tion was conducted on a GPC system followed by a thorough clean - up with H2SO4. The separation was performed on an HP -5ms capillary column. Identification and quantification were conducted using GC -ECD. Toxaphene concen- tration exhibited a good linearity over the range of 20 -500 μg/L with R≥0.998. The detection limit of this method was 1.0 μg/kg for toxaphene. The recovery rates of toxaphene were 73.7% -78.7% at the range of 2.0 -20.0 μg/kg. This accurate and sensitive method can be applied for the determination of toxaphene residues in aquatic products.

关 键 词：气相色谱 毒杀芬 水产品 残留 电子捕获检测器 

分 类 号：S948[农业科学—水产养殖]