液相色谱串联质谱法测定中药材原料中154种农药残留  

Analysis of 154 Pesticides Residues in Traditional Chinese Medicinal Materials by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：耿春辉 张嘉楠 王爱卿 周凤盈 崔婧 韩吉祥 GENG Chunhui;ZHANG Jianan;WANG Aiqing;ZHOU Fengying;CUI Jing;HAN Jixiang(Hengshui Comprehensive Inspection and Testing Center,Hengshui 053000,China;Agricultural Products Quality Inspection Center of Qinhuangdao City,Qinhuangdao 066000,China;Cangzhou Agricultural Product Quality and Safety Center,Cangzhou 061000,China)

机构地区：[1]衡水市综合检验检测中心,河北衡水053000 [2]秦皇岛市农产品质量安全检验监测中心,河北秦皇岛066000 [3]沧州市农产品质量安全中心,河北沧州061000

出　　处：《特产研究》2024年第6期132-143,164,共13页Special Wild Economic Animal and Plant Research

基　　金：河北省市场监督管理局科研计划项目(2021ZD40,2022ZD37)。

摘　　要：为提高中药材原料中农药多残留检测的效率及准确性。本研究建立了基于全自动QuEChERS方法的中药材原料中154种农药残留量的液相色谱-串联质谱(LC-MS/MS)快速检测技术,对前处理条件和仪器条件进行了优化,并进行了基质效应评价。中药磨粉后加水浸润,采用1%(v/v)乙酸乙腈提取,采用全自动QuEChERS设备进行提取和净化,净化液过0.22μm有机滤膜过滤后,采用LC-MS/MS在多反应监测(MRM)模式下测定,基质匹配外标法定量。结果表明,154种农药在2.0~100.0μg/L的线性范围内,相关系数(R)均大于0.999,定量限均可达到0.01mg/kg,在0.01、0.02、0.10 mg/kg的加标水平下,回收率分别为60.7%~96.2%、68.3%~93.5%、64.2%~97.5%,相对标准偏差(RSD)分别为0.4%~8.3%、0.3%~4.9%、1.0%~10.4%。应用所建立的方法对本地自产及市售的56批中药原料进行测定,结果表明,有27批中药原料中检出农药残留,共检出45种农药,包括药典中禁用的农药杀虫脒、特丁硫磷以及克百威。该方法简便、快速、自动化程度高,适用于中药原料中农药多残留的快速分析。In order to improve the efficiency and accuracy of pesticide residue detection in raw materials of troditional Chinese medicinal materials.To establish a rapid method for the determination of 154 kinds of pesticide residues in traditional Chinese medicinal materials by liquid chromatography-tandemmass spectrometry(LC-MS/MS)combined with automatic QuEChERS.The pretreatment conditions and instrument conditions were optimized and the matrix effect was evaluated.The samples were added with water,then extracted with acetonitrile containing 1%(v/v)acetic acid,extracted and purified with automatic QuEChERS equipment,the purified solution is filtered through the filter membrane,and determined by LC-MS/MS in multi-reaction monitoring(MRM)mode and quantified by matrix matching external standard method.The linearities of 154 kinds of pesticides ranged from2.0~100.0 μg/L,with correlation coefficients more than 0.999.The results showed that the recoveries for all compounds spiked at levels of 0.01、0.02、0.10 μg/kg,which were 60.7%~96.2%,68.3%~93.5%,and 64.2%~97.5%respectively,with relative standard deviations(RSDs)were 0.4%~8.3%、0.3%~4.9%、1.0%~10.4%.The method was applied to the determination of 56 batches of traditional Chinese medicinal materials.The results showed that pesticide residues were detected in 27 batches of traditional Chinesemedicinalmaterials,and a total of 45 pesticides were detected,including the banned pesticides chlordimeform,terbufos and carbofuran in the Chinese pharmacopoeia.Therefore,the developed method was simple,rapid,sensitive and automatic,and was suitable for the rapid detection of pesticide residues in traditional Chinese medicinal materials.

关 键 词：中药材 农药多残留分析 全自动QuEChERS 液相色谱串联质谱法 

分 类 号：R284[医药卫生—中药学] O657.63[医药卫生—中医学]