王朝杰　李倩　胡玉霞　张友青　杨娜

摘要 建立了蔬菜中有机氯类农药残留量的固相萃取—毛细管气相色谱（SPE-CGC）分析方法。对蔬菜中六六六的4 种异构体、滴滴涕的4 种异构体、乙烯菌核利、α-硫丹、β-硫丹、腐霉利、异菌脲、氯菊酯等14 种有机氯农药的残留量进行了测定。以丙酮-正己烷混合物超声波提取样品，采用HP-5毛细管气相色谱柱分离样品，ECD测定。结果表明，在所建立的方法下，14种有机氯农药能够很好地分离，峰面积与其质量浓度有良好的线性关系，检出限在0.000 1～0.001 0 mg/kg范围内，加标回收率在78.25%～96.55%之间，相对标准偏差均在0.55%～2.91%。该法简单、快捷、灵敏、准确，可用于日常蔬菜中大部分有机氯农药残留的测定。

关键词 固相萃取—毛细管气相色譜法；蔬菜；有机氯农药；残留量

中图分类号 S63；O657.8 文献标识码 A 文章编号 1007-5739（2016）05-0137-03

Abstract The solid-phase extraction and capillary gas chromatography was introduced for determining 14 organochlorine pesticide residues including α-benzene hexachloride（BHC），β-BHC，γ-BHC，δ-BHC，p，p′-dichloro-diphenyl-dichloroethylene（PP′-DDE），pp′-dichloro-diphenyl-dichloroethane（PP′-DDD），o，p′-dichloro-diphenyl-trichloroethane（OP′-DDT），PP′-DDT，vinclozolin，α-endosulfan，β-endosulfan，procymidone，iprodione，permethrin.The organochlorine pesticides were extracted from vegetables with mixed solvents of acetone and n-hexane by ultrasonic and purified by florisil solid phase extraction column. Then，the extract was separated by HP-5 capillary column and detected by electrochemical detector. The results indicated that the 14 organochlorine pesticides were well separated，the good linearities were obtained，the detection limits were between 0.000 1～0.001 0 mg/kg，the average recoveries were between 78.25 %～ 96.55% and relative standard deviations of 0.55%～2.91%.The method is simple，rapid，accurate and highly sensitive，and it can be used for the simultaneous determination most of organochlorine pesticide residuals in vegetables.

Key words solid-phase extraction and capillary gas chromatography；vegetables；organochlorine pesticides；residuals

有机氯类农药作为高效杀虫剂，广泛使用于蔬菜种植养护中，在环境中容易造成残留进入食物链而影响人体健康。我国是蔬菜生产和消费大国，而蔬菜中毒事件屡屡发生[1-6]。因此，蔬菜中农药残留情况一直是当前各级农业行政主管部门农产品监测的重点和城乡居民关注的热点，并成为制约我国蔬菜及其制品出口的主要问题[7]。解决这一难题的关键是如何更快、更有效地通过检测控制农药残留量问题。因此，分析的质量必须符合特定的要求，并且力求易操作、快速、简便、溶剂使用少、低成本、低污染等[8-9]。

笔者以我国“农业行业标准”方法为基础，用毛细管气相色谱外标法对α-BHC、β-BHC、γ-BHC、δ-BHC、乙……