中草药中40种农药残留的气相色谱-质谱分析  

Multi-residues Analysis of Pesticides in Herbal Medicines by Gas Chromatography-mass Spectrometry with SIM Model

作　　者：聂春林[1] 吴海[1] 梁逸曾[1] 

机构地区：[1]中南大学中药现代化研究中心

出　　处：《精细化工中间体》2008年第4期59-65,共7页Fine Chemical Intermediates

基　　金：科技部国际科技合作项目(2006DFA41090;2007DFA40680)

摘　　要：建立了一种同时测定中草药中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯等四大类40种农药残留量的分析方法。通过比较三氯甲烷、乙腈、正己烷、乙酸乙酯和丙酮等多种溶剂的提取效果,确定三氯甲烷和丙酮为提取溶剂;提取的样品经弗罗里硅土净化,用GC-MS选择离子模式进行测定,采用外标法进行定量。40种农药在65min内达到理想的分离效果。以2个添加水平测定样品的回收率和相对标准偏差,回收率在88.6%和107.1%之间,RSD均低于8.0%。各农药检测限为0.5～37.5μg/kg,定量限为1.4～112.5μg/kg。采用该方法,对百合、刀豆、菊花、黄芪、人参、当归、车前草7种不同种类的中草药进行了实际检测,均发现一定量的农药残留。该方法简便、快速、准确、灵敏,且重现性好,可用于中草药中多种农药残留的同时测定。An analysis method based on gas chromatography-mass spectrometry （GC-MS） was developed to determine 40 pesticides including organochlorinates, organophosphates, synthetic pyrethroids and carbamate. Sample was extracted with mixture of chloroform and acetone and the extract was further purified through a Florisile column chromatography. The prepared sample was then analyzed using GC-MS with selective ion monitoring （SIM） mode. 40 pesticides were well separated within 65 minutes, and all relative standard deviations （RSD） were less than 8.0%, and the recoreries were 88.6%-107.5%. The limits of detection （LODs） ranged ratio 3：1, and the limits of quantitation （LOQs） were 1.4-112.5μg/kg. The good repeatability. It is suitable for the multiresidues analysis of pesticides in from 0.5-37.5μg/kg under the signal noise method is simple, rapid, sensitive, and of herbal medicines.

关 键 词：气相色谱-质谱法 中草药 多农药残留 

分 类 号：S481.8[农业科学—农药学]