GPC净化-GC-MS/MS法测定鳗鱼中杀虫脒、双甲脒及代谢物残留  

Determination of Chlordimeform, Amitraz and Their Metabolity Residues in Eel by GC-MS/MS with GPC Purification

作　　者：刘海燕[1] 刘针铃 任民红[1] 吕蓉[1] 左海根[1] 郭平[1] 

机构地区：[1]江西出入境检验检疫局检验检疫综合技术中心,南昌330000

出　　处：《食品工业》2015年第12期255-258,共4页The Food Industry

基　　金：江西省青年科学基金项目(20142BAB213028)

摘　　要：建立了鳗鱼中杀虫脒及其代谢物4-氯邻甲基苯胺、双甲脒及其代谢物2,4-二甲基苯胺残留的GPC-GC/MS/MS检测方法。样品经环己烷＋乙酸乙酯（1＋1）均质提取,凝胶渗透色谱净化,采用气相色谱-串联质谱检测,外标法定量。结果表明：4种农药在5~100μg/L质量浓度范围内,组分含量与峰面积呈线性相关,相关系数为0.998 8~0.999 8,4种农药在鳗鱼中不同质量浓度水平的加标回收率分别为74.55%~99.28%,71.09%~96.70%和77.47%~89.42%,相应的相对标准偏差分别为2.52%~4.49%,2.78%~5.27%和0.73%~3.27%（n=6）。方法检出限为0.07~2.0μg/kg。该方法具有检出限低、灵敏度高、快速、准确的特点,可适用于鳗鱼中杀虫脒、双甲脒及代谢物农药残留同时检测。It was an analytical method for the determination of chlordimeform and its metabolite 4-chloro-2-methyl aniline, amitraz and its metabolite 2, 4-dimethyl aniline were in Eel by GC-MS/MS with GPC Purification. Samples were treated by homogenization extraction with cyclohexane ＋ethyl acetate（1＋1） and gel permeation chromatography（GPC）. The analysis was performed by gas chromatography-tandem mass spectrometry detection and the external standard of legal measures. The linearity of the method ranged from 5 to 100 μg/L, with correlation coefficients ranging from 0.998 8 to 0.999 8. The recovery of standard addition of 4 kinds of pesticides in different concentration levels in eel rate respectively was 74.55%~99.28%, 71.09%~96.70% and 77.47%~89.42%. The relative standard deviation of the corresponding respectively was 2.52%~4.49%, 2.78%~5.27% and 0.73%~3.27%（n=6）. The detection limit was 0.07~2.0 μg/kg. The method had low detection limit, high sensitivity, rapid and accurate, could be used for simultaneous detection of residues in eel on pesticide chlordimeform, amitraz and its metabolite.

关 键 词：凝胶渗透色谱(GPC) 气相色谱-串联质谱(GC-MS/MS) 杀虫脒 双甲脒 2 4-二甲基苯胺 4-氯邻甲基苯胺 鳗鱼 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]