气相色谱-质谱法测定蜂王浆中杀虫脒及其代谢产物残留量

Determination of Residues of Chlordimeform and Metabolites in Royal Jelly by Gas Chromatography Mass-Spectrometry

建立了蜂王浆中杀虫脒及其代谢产物残留量的气相色谱-质谱分析方法,并对样品预处理的方法和定量检测条件作了较详细的探讨。样品经过三氯乙酸进行蛋白质沉淀处理,在碱性条件下用正己烷-丙酮(5+5,v/v)溶剂提取,提取液经正己烷、乙腈液液分配净化后,气相色谱-质谱检测和确证,外标法定量。杀虫脒和4-氯邻甲苯胺的室内回收率分别为81.2%～112%,79.4%～109%。方法的测定低限为0.01mg/kg。

A gas chromatography-mass spectrometric method for the determination of residues of chlordimeform and its metabolite of 4-chloro-2-methylaniline in royal jelly was developed. The operating conditions for determination of residues were investigated in detail. The protein in royal jelly was precipitated by trichloroacetic acid, and the residues were extracted with n-hexane-acetone （5 ＋5, v/v） under alkaline conditions. After the liquid-liquid partition with n-hexane-acetonitrile, the residues were determined by gas chromatography-mass spectrometry with external standard method. The recovery ranges of chlordimeform and 4-chloro-2-methylaniline were 81.2%-112%, 79.4%-109%, respectively. The limit of detection of chlordimeform and 4-chloro-2-methylaniline was 0.01 mg/kg.