固相萃取-高效液相色谱-串联质谱联用法快速测定中药材猴耳环中47种农药残留  

Rapid determination of 47 pesticide residues in Folium Archidendri by SPEhigh performance liquid chromatography-tandem mass spectrometry

作　　者：李纯[1] 熊颖[1] 顾利红[1] 侯惠婵[1] 栗建明[1] LI Chun;XIONG Ying;GU Lihong;HOU Huichan;LI Jianming(NMPA Key Laboratory for Quality Evaluation of Traditional Medicine,Guangzhou Institute for Drug Control,Guangzhou 510160,China)

机构地区：[1]广州市药品检验所,国家药品监督管理局中成药质量评价重点实验室,广州510160

出　　处：《农药学学报》2021年第1期183-188,共6页Chinese Journal of Pesticide Science

基　　金：国家药典委员会药品标准研究课题(2018Z011-专项).

摘　　要：建立了固相萃取-高效液相色谱-串联质谱同时检测中药材猴耳环中47种农药残留的方法。样品经乙腈高速匀浆提取,亲水亲油平衡材料(简称HLB)固相萃取柱净化,采用电喷雾正离子扫描(ESI+)、依赖保留时间的多反应监测模式(scheduled MRM)测定,基质匹配标准溶液外标法定量。结果表明:47种农药在各自线性范围内其质量浓度与峰面积间呈良好线性关系(r>0.9920),定量限在0.001~0.015 mg/kg之间,平均回收率在54%~117%之间,RSD在2.0%~15%之间,其中40种农药的平均回收率在70%~120%之间,满足痕量分析要求。该法操作简便快捷,稳定性好,灵敏度高,适用于猴耳环中农药多残留的监控与筛查。In this work,a method was developed for the determination of 47 pesticide residues in Folium Archidendri using HLB solid phase extraction by high performance liquid chromatographytandem mass spectrometry(HPLC-MS/MS).Electrospray ionization source was applied by positive ionization(ESI+)in scheduled multiple reaction monitoring modes.The samples were extracted with acetonitrile by high speed homogenizer,purified by HLB SPE,and analyzed quantitatively by matrixmatched external standard curve method.The calibration curves of 47 targets showed good linearity with correlation coefficients of above 0.9920.The average recoveries were in the range of 54%-117%,with RSDs of 2.0%-15%.LOQs of all the tested pesticides were 0.001-0.015 mg/kg.Among them,the recoveries of 40 pesticides were in the range of 70%-120%,which met the requirements of multipesticides trace analysis.This analytical method was simple,quick,stable and sensitive,which could be used for a monitoring and screening analysis of multi-pesticide residues in Folium Archidendri.

关 键 词：固相萃取 高效液相色谱-串联质谱 猴耳环 农药多残留 中药材 

分 类 号：TQ450.2[化学工程—农药化工] X592[环境科学与工程—环境工程]