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基质固相分散萃取-高效液相色谱串联质谱法(HPLC-MS-MS)同时测定茶叶中11种农药的残留量

  • 刘妍慧 ,
  • 于常红 ,
  • 刘岩 ,
  • 刘健 ,
  • 张婷
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  • 1. 中国海洋大学环境科学与工程学院,山东 青岛 266100;
    2. 中国海洋大学海洋环境与生态教育部重点实验室,山东 青岛 266100;
    3. 青岛大学医学院,山东 青岛 266071;
    4. 山东省科学院海洋仪器仪表研究所 山东省海洋环境监测技术重点实验室,山东 青岛 266001
刘妍慧(1992— ),女,浙江诸暨人,主要从事环境科学与环境污染监测/检测研究。

收稿日期: 2013-09-02

  修回日期: 2013-10-21

  网络出版日期: 2019-09-03

基金资助

青岛市科技发展计划项目(13-1-3-129-nsh)、山东省自然科学基金(ZR2013DL008)、山东省高等学校科技计划项目(J11LF20)、山东省优秀中青年科学家科研奖励基金(BS2011YY001)

Simultaneous Determination of 11 Kinds of Pesticide Residues in Tea by HPLC-MS-MS

  • LIU Yanhui ,
  • YU Changhong ,
  • LIU Yan ,
  • LIU Jian ,
  • ZHANG Ting
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  • 1. College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China;
    2. Key Lab of Ocean Environment and Ecology, Ministry of Education, Ocean University of China, Qingdao 266100, China;
    3. Medical School,Qingdao University, Qingdao 266071, China;
    4. Shandong Provincial Key Laboratory of Ocean Environment Monitoring Technology, Institute of Oceanographic Instrumentation, Shandong Academy of Sciences, Qingdao 266001, China

Received date: 2013-09-02

  Revised date: 2013-10-21

  Online published: 2019-09-03

摘要

建立了茶叶中3类11种农药的分散固相萃取–高效液相色谱串联质谱(HPLC-MS-MS)的检测方法。茶叶样品以乙腈–乙酸(体积比99:1)提取,以PSA为净化剂基质固相分散萃取,然后通过C18色谱柱,以甲醇/水(含甲酸铵)溶液进行梯度洗脱,采用电离喷雾电离方式(ESI+),通过多反应监测(MRM)定量。结果表明:11种农药的分析时间约为20 min,在0~500 ng·mL-1范围内线性相关,相关系数大于0.9995,方法检测限为0.1~1.7 μg·kg-1。测定了茶叶样品中11种农药的残留量,加标回收率为62.4%~114.8%(添加水平分别为10~400 μg·kg-1),相对标准偏差(RSD)为3.28%~19.34%。选取了5个不同类型的茶叶样品,检测其中11种农药的残留量,检出结果差异较大。其中绿茶中11种农药的检出量为1.7~339.4 μg·kg-1,加标回收率为86.1%~104.1%,相对标准偏差(RSD)均小于20%(n=6)。本方法准确、灵敏、简单、快速、安全,能满足茶叶样品中多种农药残留分析的要求。

本文引用格式

刘妍慧 , 于常红 , 刘岩 , 刘健 , 张婷 . 基质固相分散萃取-高效液相色谱串联质谱法(HPLC-MS-MS)同时测定茶叶中11种农药的残留量[J]. 茶叶科学, 2014 , 34(3) : 271 -278 . DOI: 10.13305/j.cnki.jts.2014.03.009

Abstract

A method for rapid determination of 11 kinds of pesticide residues in tea samples by matrix solid-phase disperse extraction and high performance liquid chromatography and tandem mass spectrometry was proposed. The pesticide residues in tea sample were firstly extracted by a mixture of V(acetonitrile):V(acetic acid)=99:1, and the extract was solid-phase disperse purified by PSA and then separated on a Waters Xterra MS C18 column with a gradient system of a mixture of methanol and water with ammonium formate. Multi-reaction monitoring (MRM) was employed for quantitative determination. Eleven pesticide residues could be detected within 20 min. The linear range of 11 pesticide residue was 0-500 ng·mL -1 and the limits of detection were between 0.1-1.7 μg·kg-1. The correlation rate was more than 0.9995. The average recoveries (spiked at the levels of 10-400 μg·kg-1) ranged from 62.4% to 114.8% with relative standard deviation between 3.28% and 19.34%. After extraction and purification, 11 pesticide residues in 5 samples of different kinds of tea with significant variation in content were analyzed. And the residue content of 11 pesticides in green tea sample was 1.7-339.4 μg·kg-1. Recoveries in this sample were ranged from 86.1% to 104.1% with relative standard deviations less than 20%. This method is accurate, sensitive, simple, rapid,safe and suitable for identification and quantification of multiple pesticide residues in tea.

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