高效液相色谱-柱后衍生-荧光检测器测定中药材中13种氨基甲酸酯类农药残留

HPLC for the simultaneous determination of 13 pesticides in traditional Chinese herbal medicines

目的:研究中药材中13种氨基甲酸酯农药多残留的测定方法。方法:采用高效液相色谱-柱后衍生法,荧光检测器,激发波长为330nm,发射波长为465nm。前处理方法为乙腈高速均质匀浆的提取方法和固相萃取柱(SPE)的净化方法。结果:考察了6种不同的中药材样品基质、在3水平添加条件下,13种农药的回收率在74.1%～108.8%,相对标准偏差小于15%,检测限在0.0003～0.06mg/kg。结论:测定方法经复核表明,重现性良好,可作为中药材中氨基甲酸酯类农药多残留测定的方法。

AIM：To study a method for the determination of 13 N-methylcarbamate peticides in traditional Chinese herbal medicines（TCHMs）.METHODS：Thirteen pesticides were extracted by acetonitrile,and purified through solid phase extraction（SPE） cartridges,then detected by HPLC with post-column derivatization and Fluorescense Detector excited wavelength was 330 nm,emissive wavelength was 465 nm.RESULTS：The analytical performance was demonstrated by the analysis of 6 TCHMs samples＇extracts,spiked at three concentration levels for each pesticide.In general,the recoveries ranging from 74.1 to 108.8%,with relative standard deviations（RS-Ds） better than 15%,were obtained.The limit of quantification（LOD） of 13 pesticides from 0.000 3 to 0.06 mg/kg.CONCLUSION：The method has good extraction efficiency and purification effect,which could be standard of N-methylcarbamate peticides residues in the routine analysis of TCMs.