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QuEChERS-气相色谱三重四极杆串联质谱法测定土壤中227种农药残留

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贺泽英, 张艳伟, 王雯雯, 吕美玲, 徐亚平. QuEChERS-气相色谱三重四极杆串联质谱法测定土壤中227种农药残留[J]. 环境化学, 2020, (7): 2022-2025.
引用本文: 贺泽英, 张艳伟, 王雯雯, 吕美玲, 徐亚平. QuEChERS-气相色谱三重四极杆串联质谱法测定土壤中227种农药残留[J]. 环境化学, 2020, (7): 2022-2025.
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HE Zeying, ZHANG Yanwei, WANG Wenwen, LYU Meiling, XU Yaping. Analysis of 227 pesticide residues in soil using QuEChERS combined with gas chromatography-triple quadrupole mass spectrometry[J]. Environmental Chemistry, 2020, (7): 2022-2025.
Citation: HE Zeying, ZHANG Yanwei, WANG Wenwen, LYU Meiling, XU Yaping. Analysis of 227 pesticide residues in soil using QuEChERS combined with gas chromatography-triple quadrupole mass spectrometry[J]. Environmental Chemistry, 2020, (7): 2022-2025.
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QuEChERS-气相色谱三重四极杆串联质谱法测定土壤中227种农药残留

  • 1. 农业农村部农产品质量安全环境因子控制重点实验室, 国家农业检测基准实验室(农药残留), 农业农村部环境保护科研监测所, 天津, 300191;

  • 2. 安捷伦科技(中国)有限公司, 北京, 100102

    • 通讯作者: 徐亚平, E-mail: nyhjzxtj@163.com
  • 基金项目:

    国家重点研发计划（2016YFD0201203）资助.

Analysis of 227 pesticide residues in soil using QuEChERS combined with gas chromatography-triple quadrupole mass spectrometry

  • 1. Key Laboratory for Environmental Factors Control of Agro-product Quality Safety, National Reference Laboratory for Agricultural Testing P. R. China, Ministry of Agriculture, Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin, 300191, China;

  • 2. Agilent Technologies(China) Company, Ltd., Beijing, 100102, China

    • Corresponding author: XU Yaping, nyhjzxtj@163.com
  • Fund Project: Supported by the National Key R&D Program (2016YFD0201203).

  • 摘要: 本文开发了基于QuEChERS前处理结合气相色谱三重四极杆串联质谱检测土壤中227种农药残留的高通量方法.对QuEChERS前处理的提取方式、提取时间、缓冲盐、净化条件等参数进行了优化，在最优条件下进行了方法学考查.结果表明，227种农药在2-200 μg·L-1的范围内，线性良好，绝大部分农药的线性相关系数大于0.99；农药回收率在70%-120%之间，相对标准偏差<20%.根据不同添加浓度下的准确度和精密度数据确定了本方法的定量限在2-20 μg·kg-1之间，78.4%的农药定量限可低至2 μg·kg-1.最后将方法用于实际样品的检测.该方法简单、快速、重现性好、灵敏度高，可满足土壤中农药残留的大批量快速筛查和准确定量分析.
    Abstract: Quick and high efficient multiresidue analysis method is critical for screening and moniotring of the pesticide residue in soil. In this study, a high throughput multiresidue method was developed based on QuEChERS sample preparation method combined with gas chromatography-triple quadrupole mass spectrometry. The extraction and clean-up procedures and parameters including extraction method, extraction time, buffer system, and clean-up adsorbent selection were thoroughly investigated and optimized. Most coefficients of determination (r2) were higher than 0.99 within the calibration linearity range of 2-200 μg·L-1. Most recoveries at six spiking levels were in the range of 70%-120% with RSDs <20% indicating satisfactory accuracy. The limits of quantification (LOQ) for the pesticides were determined based on recovery and accuracy results and ranged from 2 to 20 μg·kg-1, and for 78.4% of the pesticides the LOQs were 2 μg·kg-1. Finally, the proposed method was used in real sample analysis. This method was proved to be simple, sensitive and effective, which can be applied for large-scale pesticide screening and quantification in soils.
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  • [1] 张璐, 张亚莉, 何强, 等. 超高液相色谱/线性离子阱-静电场轨道阱高分辨质谱法快速筛查土壤中氨基甲酸酯类农药残留量[J]. 分析试验室, 2017, 36(1):60-65.

    ZHANG L, ZHNAG Y L, HE Q, et al. Determination of 23 carbamate pesticide residues in soil by ultra-performance liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry[J]. Chinese Journal of Analysis Laboratory,2017, 36(1):60-65(in Chinese).

    [2] JOSE F, PILAR H N,MARTNEZ C M, et al. Multiresidue analysis of pesticides in soil by high-performance liquid chromatography with tandem mass spectrometry[J]. Journal of AOAC International, 2019, 92(5):1566-1575.
    [3] ANASTASSIADES M, LEHOTAY S J, STAJNBAHER D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce[J]. Journal of AOAC International, 2003, 86(2):412-431.
    [4] CEN. Foods of plant origin-detetrmination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE-QuEChERS-method[S]. BS EN 15662:2008.
    [5] AOAC, Pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate[S]. AOAC official method 2007.01.
    [6] FENG X, HE Z Y, WANG L, et al. Multiresidue analysis of 36 pesticides in soil using a modified quick, easy, cheap, effective, rugged, and safe method by liquid chromatography with tandem quadruple linear ion trap mass spectrometry[J]. Journal of Separation Science, 2015, 38(17):3047-3054.
    [7] YU Y, LIU X W, HE Z Y, et al. Development of a multi-residue method for 58 pesticides in soil using QuEChERS and gas chromatography-tandem mass spectrometry[J]. Analytical Methods, 2016, 8(11):2463-2470.
    [8] 尹君, 马琳, 黄兰淇,等. QuEChERS/超高效液相色谱-串联质谱法同时测定土壤中67种农药残留[J]. 分析测试学报, 2018,37(5):562-569.

    YI J, MA L, HUANG L Q, et al. Simultaneous determination of 67 pesticide residues in soil by QuEChERS/Ultra high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Instrumental Analysis, 2018,37(5):562-569(in Chinese).

    [9] 蔡霖, 席普宇, 谢晴,等. QuEChERS方法联合HPLC-MS/MS和GC-MS测定土壤中110种农药残留[J]. 农业环境科学学报, 2017,36(8):1680-1688.

    CAI L, XI P Y, XIE Q, et al. Development of a multiresidue method for determination of 110 pesticide residues in soil using QuEChERS-HPLC-MS/MS and QuEChERS-GC-MS[J]. Journal of Agro-Environment Science, 2017,36(8):1680-1688(in Chinese).

    [10] HE Z Y,WANG Y H,WANG L, et al. Determination of 255 pesticides in edible vegetable oils using QuEChERS method and gas chromatography tandem mass spectrometry[J]. Analytical & Bioanalytical Chemistry, 2017,409:1017-1030.
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QuEChERS-气相色谱三重四极杆串联质谱法测定土壤中227种农药残留

    通讯作者: 徐亚平, E-mail: nyhjzxtj@163.com
  • 1. 农业农村部农产品质量安全环境因子控制重点实验室, 国家农业检测基准实验室(农药残留), 农业农村部环境保护科研监测所, 天津, 300191;
  • 2. 安捷伦科技(中国)有限公司, 北京, 100102
基金项目:

国家重点研发计划（2016YFD0201203）资助.

摘要: 本文开发了基于QuEChERS前处理结合气相色谱三重四极杆串联质谱检测土壤中227种农药残留的高通量方法.对QuEChERS前处理的提取方式、提取时间、缓冲盐、净化条件等参数进行了优化，在最优条件下进行了方法学考查.结果表明，227种农药在2-200 μg·L-1的范围内，线性良好，绝大部分农药的线性相关系数大于0.99；农药回收率在70%-120%之间，相对标准偏差<20%.根据不同添加浓度下的准确度和精密度数据确定了本方法的定量限在2-20 μg·kg-1之间，78.4%的农药定量限可低至2 μg·kg-1.最后将方法用于实际样品的检测.该方法简单、快速、重现性好、灵敏度高，可满足土壤中农药残留的大批量快速筛查和准确定量分析.

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