Objective To establish an analytical method for detecting hexachlorocyclohexane, dichlorodiphenyltrichloroethane, endosulfan, heptachlor, chlordane, aldrin, dieldrin, endrin and their metabolites residues in traditional Chinese medicinal herbs including plumeria, dried date, ginseng, dangshen, radix ginseng rubra, cordate houttuynia and astragalus with gel permeation chromatography-solid phase extraction-gas chromatography method. Methods Traditional Chinese medicinal herbs were crushed and immersed in deionized water, extracted with ethyl acetate and acetone (1:1, v:v), and then purified by gel permeation chromatography and solid phase extraction, and detected by gas chromatography (with μECD detector). Results The linear range of those 17 organo-chlorine pesticides were from 10 to 100 µg/mL with the correlation coefficients (R) more than 0.999. The recoveries of the 17 compounds ranged from 84.6% to 115.5%with the relative standard deviation (RSD, n=6) lower than 14.5%, and the limit of quantitation (LOQ) of the method ranged from 0.31 to 4.15 µg/kg. Conclusions The experimental method was simultaneous, accurate, efficient, environmentally friendly, and suitable for the rapid detection of 17 organochlorine pesticides in traditional Chinese medicinal herbs.%目的：建立基于凝胶渗透色谱(gel permeation chromatography, GPC)和固相萃取(solid phase extraction, SPE)净化技术的药食两用植物性中药材(鸡蛋花、干枣、人参、丹参、高丽红参、鱼腥草、黄芪、枸杞、菊花、玉竹、凉粉草、西洋参、百合)中六六六,滴滴涕,硫丹,七氯,氯丹,艾氏剂,狄氏剂及异狄氏剂17种有机氯农药残留的气相色谱检测方法。方法中药材粉末经去离子水浸泡,乙酸乙酯和丙酮(1：1, v：v)提取,凝胶渗透色谱初步净化,石墨化碳黑和氨基固相萃取柱进一步净化,气相色谱仪(带µECD检测器)进行检测。结果该方法中17种化合物在10~100µg/kg范围内线性良好,相关系数R>0.999,在三个水平添加回收试验中,17种化合物的回收率在84.6%~115.5%之间,相对标准偏差(RSD, n=6)为3.1%~14.5%。该方法的定量限(LOQ)介于0.31~4.15µg/kg。结论该方法具有准确、灵敏、高效、环保的特点,适用于中药材中17种有机氯类农药的同时快速检测。
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