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超高效液相色谱-静电场轨道阱高分辨质谱法测定茶叶中21种农药残留量

  • 金莉莉 ,
  • 郝振霞 ,
  • 高贯威 ,
  • 柴云峰 ,
  • 王晨 ,
  • 陈红平 ,
  • 鲁成银
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  • 1. 中国农业科学院茶叶研究所 农业部茶叶产品质量安全风险评估实验室(杭州),农业部茶叶质量安全控制重点实验室,浙江 杭州 310008;
    2. 中国农业科学院研究生院,北京 100081
金莉莉,女,硕士研究生,主要研究方向为茶叶质量安全检测与研究。

收稿日期: 2018-03-06

  修回日期: 2018-04-23

  网络出版日期: 2019-12-15

基金资助

中国农业科学院创新团队茶叶质量与风险评估团队(CAAS-ASTIP-2014-TRICAAS-06)、国家自然科学基金项目(31601554)、浙江省自然科学基金项目(LQ16C200006)、浙江省公益应用项目(2017C32059)、现代农业产业技术体系建设专项基金资助项目(nycytx-26)

Determination of 21 Pesticide Residues in Tea by Ultra Performance Liquid Chromatography Orbitrap High Resolution Mass Spectrometry

  • JIN Lili ,
  • HAO Zhenxia ,
  • GAO Guanwei ,
  • CHAI Yunfeng ,
  • WANG Chen ,
  • CHEN Hongping ,
  • LU Chengyin
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  • 1. Tea Research Institute, Chinese Academy of Agricultural Sciences, Laboratory of Quality and Safety Risk Assessment for Tea Products (Hangzhou), Key Laboratory of Tea Quality and Safety Control, Ministry of Agriculture, Hangzhou 310008, China;
    2. Chinese Academy of Agricultural Sciences, Beijing 100081, China

Received date: 2018-03-06

  Revised date: 2018-04-23

  Online published: 2019-12-15

摘要

采用超高效液相色谱-静电场轨道阱高分辨质谱,建立了茶叶中21种农药残留量的检测方法。茶叶样品经甲醇和水(V甲醇V=1∶1)提取后,采用乙二胺-N-丙基硅烷和强阳离子交换剂作为混合吸附剂进行萃取净化。以C18色谱柱进行色谱分离,采用Full Scan扫描模式进行定性、定量分析。结果显示,21种农药在0.5~200βμg·L-1范围内均呈良好的线性关系,相关系数(r2)大于0.99。在10、50、100βμg·kg-1 3个加标水平下,平均回收率为70%~125%之间,相对标准偏差(RSD)小于15%,定量限为10βμg·kg-1。本方法操作简单快速,灵敏度高,适用于茶叶中21种农药残留检测。

本文引用格式

金莉莉 , 郝振霞 , 高贯威 , 柴云峰 , 王晨 , 陈红平 , 鲁成银 . 超高效液相色谱-静电场轨道阱高分辨质谱法测定茶叶中21种农药残留量[J]. 茶叶科学, 2018 , 38(6) : 595 -605 . DOI: 10.13305/j.cnki.jts.2018.06.006

Abstract

A ultra performance liquid chromatography orbitrap high resolution mass spectrometry method for the determination of 21 pesticides in tea was developed. The tea samples were extracted by methanol-water (VmethanolVwater=1∶1), and cleaned up by a mixture of adsorbents containing primary secondary amine and strong cation exchanger. The chromatography analysis was performed on a C18 column. The target analytes were analyzed by high resolution mass spectrometry under Full Scan mode. The results showed that the linearities of 21 pesticides ranged from 0.5βμg·L-1 to 200βμg·L-1 with correlation coefficients higher than 0.99. At the spiked levels of 10, 50 and 100βμg·kg-1, the average recoveries were from 70% to 125%, with the relative standard deviations (RSDs) below 15%. The limits of quantitation were 10βμg·kg-1. The method is simple, rapid, sensitive and appropriate for the determination of 21 pesticide residues in tea.

参考文献

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