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改进QuEChERS/超高效液相色谱-串联质谱法同时测定当归中86种农药残留
引用本文:谢楠,张明童,刘志荣,张平,李冬华,马潇,郭朝晖,杨平荣.改进QuEChERS/超高效液相色谱-串联质谱法同时测定当归中86种农药残留[J].化学试剂,2021(2):196-203.
作者姓名:谢楠  张明童  刘志荣  张平  李冬华  马潇  郭朝晖  杨平荣
作者单位:甘肃省药品监督管理局审评认证中心;甘肃省药品检验研究院甘肃省中藏药检验检测技术工程实验室;中药材及饮片质量控制重点实验室
基金项目:甘肃省2020年度重点人才项目(2020RCXM084);甘肃省食品药品科研项目(2018GSFDA002、2019GSMPA019)。
摘    要:建立了QuEChERS结合超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定当归中86种农药残留,比较了9种不同的QuEChERS方法的净化效率和回收率,结果表明,无石墨化碳黑(NGCB)QuEChERS方法效果最佳。在依赖保留时间的多反应监测模式(MRM)下,采用UPLC-MS/MS对农药进行定量。86种农药的线性相关系数(r)均大于0.99,检出限为0.2~4μg/kg。3个添加水平(20、50、80μg/kg)下,86种农药的回收率为63.0%~130.9%,相对标准偏差(RSDs,n=6)为1.0%~18.1%。采用该方法对市场上收集的20批当归样品进行了测定,检出12种农药。该方法可为准确、高效、经济地检测当归中目标物提供参考。

关 键 词:超高效液相色谱-串联质谱(UPLC-MS/MS)  QUECHERS  农药残留  当归

Simultaneous Determination of 86 Pesticide Residues in Angelica Sinensis by Improved QuEChERS/Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry
XIE Nan,ZHANG Ming-tong,LIU Zhi-rong,ZHANG Ping,LI Dong-hua,MA Xiao,GUO Zhao-hui,YANG Ping-rong.Simultaneous Determination of 86 Pesticide Residues in Angelica Sinensis by Improved QuEChERS/Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry[J].Chemical Reagents,2021(2):196-203.
Authors:XIE Nan  ZHANG Ming-tong  LIU Zhi-rong  ZHANG Ping  LI Dong-hua  MA Xiao  GUO Zhao-hui  YANG Ping-rong
Affiliation:(Gansu Drug Administration Review and Certification Center,Lanzhou 730070,China;Gansu Tibetan Medicine Examination Engineering Laboratory,Gansu Provincial Inst让ute of Drug Control,Lanzhou 730070,China;NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine(Chinese Materia Med-ica and prepared slices),Lanzhou 730070,China)
Abstract:A method for the simultaneous determination of 86 pesticides residue in Angelica sinensis by ultra-high performance liquid chromatography/tandem mass spectrometry(UPLC-MS/MS) was established.9 kinds of QuEChERS have been compared in terms of purification efficiency and recovery,the best results were achieved with no graphitized carbon black(NGCB).The pesticides were quantified on a UPLC-MS/MS system in scheduled multiple reaction monitoring mode.Calibration curves for 86 pesticides analysts showed correlation coefficients better than 0.99.Detection limits ranged from 0.2 to 4 μg/kg.The average recoveries of 86 pesticides at the spiked levels of 20,50,80 μg/kg ranged from 63.0%~130.9% with RSDs of 1.0%~18.1%.The method was applied to the determination of 20 batches of Angelica sinensis samples collected in the market and 12 pesticides were detected.The method can provide reference for accurate,efficient and economical detection of target substances in Angelica sinensis.
Keywords:ultra-high performance liquid chromatography/tandem mass spectrometry(UPLC-MS/MS)  QuEChERS  pesticide residues  Angelica sinensis
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