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UPLC-MS/MS快速检测韭菜和土壤中氟虫腈及其代谢物残留

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贺敏, 宋丹, 董丰收, 郑永权. UPLC-MS/MS快速检测韭菜和土壤中氟虫腈及其代谢物残留[J]. 环境化学, 2016, 35(5): 925-932. doi: 10.7524/j.issn.0254-6108.2016.05.2015112002
引用本文: 贺敏, 宋丹, 董丰收, 郑永权. UPLC-MS/MS快速检测韭菜和土壤中氟虫腈及其代谢物残留[J]. 环境化学, 2016, 35(5): 925-932. doi: 10.7524/j.issn.0254-6108.2016.05.2015112002
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HE Min, SONG Dan, DONG Fengshou, ZHENG Yongquan. Determination of fipronil and its metabolites in leek and soil by ultrahigh performance liquid chromatography-mass spectrometry[J]. Environmental Chemistry, 2016, 35(5): 925-932. doi: 10.7524/j.issn.0254-6108.2016.05.2015112002
Citation: HE Min, SONG Dan, DONG Fengshou, ZHENG Yongquan. Determination of fipronil and its metabolites in leek and soil by ultrahigh performance liquid chromatography-mass spectrometry[J]. Environmental Chemistry, 2016, 35(5): 925-932. doi: 10.7524/j.issn.0254-6108.2016.05.2015112002
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UPLC-MS/MS快速检测韭菜和土壤中氟虫腈及其代谢物残留

  • 1.

    北京市农林科学院植物保护环境保护研究所, 北京, 100097;

  • 2.

    中国农业科学院植物保护研究所, 北京, 100193;

  • 3.

    长江大学农学院, 荆州, 434025

  • 基金项目:

    国家公益性行业(农业)科研专项(201303027)资助.

Determination of fipronil and its metabolites in leek and soil by ultrahigh performance liquid chromatography-mass spectrometry

  • 1.

    Institute of Plant Protection and Environment Protection, Beijing Academy of Agricultural and Forestry Science, Beijing, 100097, China;

  • 2.

    Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, 100193, China;

  • 3.

    College of Agriculture, Yangtze University, Jingzhou, 434025, China

  • Fund Project: Supported by the Special Fund for Agro-Scientific Research in the Public Interest(201303027).

  • 摘要: 建立了韭菜和土壤中氟虫腈及其代谢物的多残留分析方法.样品经乙腈提取,分散固相萃取剂净化土壤,固相萃取柱净化韭菜,超高效液相色谱-三重四极杆串联质谱在多反应离子监测模式下检测,基质匹配外标法定量.在0.001-0.2 mg·kg-1添加浓度范围内,4个化合物的平均回收率为71.8%-107.9%,相对标准偏差为1.5%-15.4%,最小检出量(LOD)在0.0001-0.012 ng范围内,土壤中最低检测浓度(LOQ)为0.001 mg·kg-1,韭菜中最低检测浓度(LOQ)为0.002 mg·kg-1.该方法满足农药残留检测的要求,适合韭菜和土壤样品中氟虫腈及其代谢物的残留检测.
    Abstract: A method was developed for the simultaneous determination of fipronil, fipronil desulfinyl, fipronil sulfone and fipronil thioether in leek and soil. The residues were extracted from samples with acetonitrile. Soil sample was cleaned up by 100 mg florisil, and leek sample was cleaned up by solid phase extraction (SPE) column. They were detected by ultrahigh performance liquid chromatography-mass spectrometry (UPLC-MS/MS) under multiple reaction monitoring mode, external standard method for quantitative by matrix-match standard solution. Average recoveries of the method ranged from 71.8%-107.9%, and the relative standard deviation was 1.5%-15.4%. The limit of detection (LOD) of these four compound were in the range of 0.0001-0.012 ng, while limit of quantification (LOQ) was 0.001 mg·kg-1 in soil and 0.002 mg·kg-1 in leek, respectively. The method was simple and reliable. It meets with the requirement of pesticide residues analysis, and could be applied for determining fipronil, fipronil desulfinyl, fipronil sulfone and fipronil thioether in leek and soil samples.
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  • 收稿日期:  2015-11-20
  • 刊出日期:  2016-05-15

UPLC-MS/MS快速检测韭菜和土壤中氟虫腈及其代谢物残留

  • 1.  北京市农林科学院植物保护环境保护研究所, 北京, 100097;
  • 2.  中国农业科学院植物保护研究所, 北京, 100193;
  • 3.  长江大学农学院, 荆州, 434025
  • 收稿日期:  2015-11-20
基金项目:

国家公益性行业(农业)科研专项(201303027)资助.

摘要: 建立了韭菜和土壤中氟虫腈及其代谢物的多残留分析方法.样品经乙腈提取,分散固相萃取剂净化土壤,固相萃取柱净化韭菜,超高效液相色谱-三重四极杆串联质谱在多反应离子监测模式下检测,基质匹配外标法定量.在0.001-0.2 mg·kg-1添加浓度范围内,4个化合物的平均回收率为71.8%-107.9%,相对标准偏差为1.5%-15.4%,最小检出量(LOD)在0.0001-0.012 ng范围内,土壤中最低检测浓度(LOQ)为0.001 mg·kg-1,韭菜中最低检测浓度(LOQ)为0.002 mg·kg-1.该方法满足农药残留检测的要求,适合韭菜和土壤样品中氟虫腈及其代谢物的残留检测.

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