气相色谱-质谱联用法同时测定中药材中53种农药残留方法

Simultaneous Determination of 53 Pesticide Residues in Traditional Chinese Herbal Medicines by GC/MS

目的采用气相色谱-质谱法研究中药材中农药多残留的测定方法。方法选用代表性的白果、人参、肉桂、红花、银杏叶、广藿香等中药材样品进行研究,样品经乙腈匀浆萃取,依次经碳十八、石墨化碳与氨丙基串联固相萃取小柱净化后,采用气相色谱-质谱同时定性、定量测定。结果在6种中药材样品基质、3水平添加条件下,53种农药的回收率大多在70.0%～120.0%,相对标准偏差小于20%,检测限大多低于0.01 mg.kg-1,符合农药多残留检测的要求。结论本法净化效果好,灵敏度高,重现性好,可用于中药材样品中农药多残留的日常检测。

OBJECTIVE To develop the multi-residues methods for traditional Chinese herbal medicines（TCHMs） by GC-MS.METHODS 6 representative samples（Semen Ginkgo,Radix Ginseng,Cortex Cinnamomi,Flos Carthami,Folium Ginkgo,and Herba Pogostemonis）were selected as experimental materials.The selected samples were extracted by acetonitrile,and then cleaned by C18 and Envi-carb/PSA solid phase extraction（SPE） cartridges.The residue detection was carried out by GC-MS.RESULTS The analytical performance was demonstrated by the analysis of 6 TCHMs samples＇ extracts,fortified at three levels for each pesticide.In general,the recoveries ranged from 70% to 120% and relative standard deviations（RSDs） were all less than 20%.The limits of detection（LODs） for most of the selected pesticides were below 0.01 mg·kg^-1.CONCLUSION The method shows high sensitivity,good repeatability and satisfactory cleaning-up excellence,which could be applied to the pesticide residue detection for the TCHMs.