摘要
建立了QuEChERS结合超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定甘草中86种农药残留,比较了9种不同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(scheduled MRM)下,采用UPLC-MS/MS法对农药进行定量。86种农药的线性相关系数(r)均大于0.9913,检出限为0.2~9μg/kg。在3个(10、50、100μg/kg)添加水平下,86种农药的回收率为65.0%~129.4%,相对标准偏差(RSD,n=6)为1.0%~19.3%。采用该方法对市场上收集的64批甘草样品进行测定,检出17种农药。该方法可为准确、高效、经济地检测甘草中目标物提供参考。
Dried Glycyrrhiza uralensis is popular as a dietary supplement in China,and it is used as an ingredient in spice and herbal medicine in China.To ensure its yields and quality,pesticides have been abused to control insects and diseases.However,the use of pesticides readily leads to pesticide residues,which may pose a potential threat to human health.To ensure that these residues are kept below tolerated levels,the China Pharmacopeia has stipulated maximum residue levels(MRLs)for some pesticides,yet only a few methods are available for evaluation of the broadly contaminated multiclass pesticides in dried Glycyrrhiza uralensis.The quick,easy,cheap,effective,rugged,and safe(QuEChERS)method,a combination of extraction and purification,has been widely accepted by the international community by virtue of providing high recovery,super efficiency,and good reproducibility.However,because of the complexity of Chinese herbal medicine matrix,QuEChERS method is not suitable for the analysis of multiclass pesticide residues.Therefore,it is urgent to establish an improved QuEChERS method for the analysis of multiple pesticide residues in Chinese herbal medicine.The method of ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established for simultaneous determination of 86 pesticides residue in Glycyrrhiza uralensis.9 kinds of QuEChERS were 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,and identified on the basis of product ion abundance ratios as well as characteristic fragments in enhanced product ion spectra UPLC-MS/MS system.The correlation coefficients of 86 analytes were better than 0.9913.Detection limits ranged from 0.2μg/kg to 9μg/kg.The average recoveries of 86 pesticides at the spiked levels of 10,50,100μg/kg were range of 65.0%-129.4%with RSDs of 1.0%-20.0%.The proposed method was applied to Glycyrrhiza uralensis samples from the Chinese market.17 pesticides were detected,including carbofuran and thiamethoxam,which exceeded the recommended maximum residue limits in some samples.The established method has advantages of good recovery,economical and a rapid clean-up procedure,showing enhanced product ion scanassisted confirmation to be a useful tool for obtaining reliable results.
作者
刘志荣
张明童
谢楠
张平
马潇
郭朝晖
LIU Zhi-rong;ZHANG Ming-tong;XIE Nan;ZHANG Ping;MA Xiao;GUO Zhao-hui(Gansu Provincial Institute of Drug Control,Lanzhou 730070,China;GanSu Tibetan Medicine Examination Engineering Laboratory,Lanzhou 730070,China)
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2020年第6期624-636,I0006,共14页
Journal of Chinese Mass Spectrometry Society
基金
甘肃省重点人才项目(2020)
甘肃省海智计划特色示范项目
甘肃省药品监督管理局科技资助项目(2018GSFDA002,2018GSFDA059,2019GSMPA019)资助。
作者简介
刘志荣(1986—),男(汉族),甘肃兰州人,工程师,从事药品质量控制研究。E-mail:553111058@qq.com;通信作者:谢楠(1976—),男(汉族),甘肃兰州人,高级工程师,从事药品质量控制研究。E-mail:7488215@qq.com。
