凝胶渗透色谱-固相萃取-气相色谱法同时测定药食两用中药材中17种有机氯类农药残留量

Determination of 17 organochlorine pesticide residues in traditional Chinese medicinal herbs by gel permeation chromatography-solid phase extraction-gas chromatography method

中文关键词:  中药材  有机氯类农药  气相色谱法  凝胶渗透色谱  固相萃取

英文关键词:traditional Chinese medicinal herbs  organochlorine pesticides  gas chromatography  gel permeation chromatography  solid phase extraction

中文摘要:

      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10~100 μg/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0.31~4.15 μg/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。

英文摘要:

      Objective To establish an analytical method for detecting hexachlorocyclohexane, dichlo-rodiphenyltrichloroethane, 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.