气相色谱法测定南美白对虾中10种拟除虫菊酯残留方法的研究  

Determination of 10 pyrethroids residues in Penaeus vannamei by gas chromatography

作　　者：母玉敏[1] 叶玫[2] 吴成业[2] 余颖[2] 邓武剑[2] 

机构地区：[1]福建农林大学食品科学学院,福建福州350002 [2]福建省水产研究所,福建厦门361012

出　　处：《上海海洋大学学报》2011年第3期399-404,共6页Journal of Shanghai Ocean University

基　　金：福建省海洋与渔业厅重点项目(闽海渔合同〔2009〕1-17号)

摘　　要：建立了气相-电子捕获检测器(GC-ECD)同时测定南美白对虾(Penaeus Vannamei)中七氟菊酯等10种拟除虫菊酯类药物残留的检测方法。样品经正己烷-乙酸乙酯-丙酮有机溶剂提取后,先采用乙腈饱和的石油醚除脂,再通过Florisil层析柱净化,最后利用GC-ECD同时测定七氟菊酯等10种拟除虫菊酯类药物残留。实验结果表明:该方法在1ng/mL^100 ng/mL浓度范围内线性良好,相关系数r≥0.999 51;在南美白对虾空白样本中加标浓度为2μg/kg、10μg/kg、20μg/kg3个水平下(七氟菊酯对应为1μg/kg、5μg/kg、10μg/kg)相应的回收率在78.0%~110.0%之间,日内精密度为4.0%~12.0%(n=6),日间精密度为2.3%~12.0%(n=3);按照10倍信噪比计算,七氟菊酯的检测限为1.0μg/kg;联苯菊酯、甲氰菊酯、三氟氯氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯、氟胺氰菊酯、氯菊酯、氟氯氰菊酯的检测限为2.0μg/kg。该方法快速、准确、可靠,适合于测定水产品中拟除虫菊酯类药物的残留。研究亮点:建立了水产品中七氟菊酯、氟胺氰菊酯、氟氯氰菊酯残留检测的气相检测方法,国内对于水产品中这3种拟除虫菊酯的气相检测研究很少。目前存在的检测方法最多可以同时检测7种拟除虫菊酯,而本课题探索出来的方法可以做到10种拟除虫菊酯同时检测。The method for determination of 10 pyrethroids residues such as tefluthrin in Penaeus vannamei by gas chromatography with electron capture detection（GC-ECD） was developed.Pyrethroids were extracted with hexan-ethylacetate-actone organic solvent and lipids were removed with petroleum ether saturated with acetonitrile.After purification by Florisil column,10 pyrethroids residues were detected simultaneously by GC-ECD.The results indicated that the working curves were linear（r≥0.999 51） in the range of 1-100 ng/mL for 10 pyrethroids.When spiked with 2 μg/kg,10 μg/kg and 20 μg/kg of pyrethroids（1 μg/kg,5 μg/kg and 10 μg/kg for tefluthrin） in Penaeus vannamei blank sample,the average recoveries were 78.0%-110.0% and the intra-day RSD（n=6） were 4.0%-12.0% and the inter-day RSD（n=3） were 2.3%-12.0%.The detection limit as estimated by 10 times signal to noise method for tefluthrin was 1.0 μg/kg and that for bifenthrin,fenpropanate,cyhalothrin,pemethrin,cyfluthrin,cypermethrin,tau-fluvalinate,fenvalate,deltamethrin was 2.0 μg/kg respectively.This method can detect pyrethroids residues in aquatic product quickly and exactly.

关 键 词：拟除虫菊酯 水产品 气相色谱法 

分 类 号：S948[农业科学—水产养殖] O657[农业科学—水产科学]