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蜂蜜中9种杀虫剂的UPLC-MS/MS检测方法

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李菊颖, 何健, 吴文铸, 孔德洋, 单正军, 陈全博. 蜂蜜中9种杀虫剂的UPLC-MS/MS检测方法[J]. 环境化学, 2016, 35(9): 1921-1927. doi: 10.7524/j.issn.0254-6108.2016.09.2016033101
引用本文: 李菊颖, 何健, 吴文铸, 孔德洋, 单正军, 陈全博. 蜂蜜中9种杀虫剂的UPLC-MS/MS检测方法[J]. 环境化学, 2016, 35(9): 1921-1927. doi: 10.7524/j.issn.0254-6108.2016.09.2016033101
shu
LI Juying, HE Jian, WU Wenzhu, KONG Deyang, SHAN Zhengjun, CHEN Quanbo. UPLC-MS/MS detection of 9 insecticides in honey[J]. Environmental Chemistry, 2016, 35(9): 1921-1927. doi: 10.7524/j.issn.0254-6108.2016.09.2016033101
Citation: LI Juying, HE Jian, WU Wenzhu, KONG Deyang, SHAN Zhengjun, CHEN Quanbo. UPLC-MS/MS detection of 9 insecticides in honey[J]. Environmental Chemistry, 2016, 35(9): 1921-1927. doi: 10.7524/j.issn.0254-6108.2016.09.2016033101
shu

蜂蜜中9种杀虫剂的UPLC-MS/MS检测方法

  • 1.

    环境保护部南京环境科学研究所国家环境保护农药环境评价与污染控制重点实验室, 南京, 210042

  • 基金项目:

    中央级公益性科研院所基本科研业务专项（农药生态影响再评估技术研究2014-002），2013年环保公益行业项目资助项目（2013467026）资助.

UPLC-MS/MS detection of 9 insecticides in honey

  • 1.

    Nanjing Institute of Environmental Science, Key Laboratory of Pesticide Environmental Assessment and Pollution Control, Ministry of Environmental Protection of the People's Republic of China, Nanjing, 210042, China

  • Fund Project: Supportd by the Central Level, Scientific Research Institutes for Basic R & D Special Fund Business(Study on the Technology of Ecological Impact Assessment of Pesticide 2014-002), Special Fund for Environmental Protection Research in the Public Interest(2013467026).

  • 摘要: 针对吡虫啉、啶虫脒、噻虫嗪、噻虫胺、噻虫啉、呋虫胺等6种新烟碱类和乐果、敌敌畏、毒死蜱等3种有机磷类杀虫剂建立了蜂蜜中分散固相萃取法-超高效液相色谱-串联质谱的残留分析方法.前处理方法利用乙腈为提取剂，N-丙基乙二胺（PSA）为分散净化剂的QuEChERS方法，并利用超高效液相色谱-串联质谱在多反应离子监测模式（MRM）下进行检测，外标法定量.结果表明，9种杀虫剂在5-800 μg·L-1浓度范围内均具有良好的线性关系（R≥0.994）；在0.005-0.200 mg·kg-1添加，水平范围内平均回收率在80.4%-107.5%之间，相对标准偏差在1.2%-6.8%之间；方法检出限（LOD）在0.1-1.5 μg·kg-1范围内；定量限（LOQ）在0.3-4.5 μg·kg-1范围内.该方法分析速度快、灵敏度高、重现性好，适用于蜂蜜中多种农药残留的快速检测和确证.
    Abstract: A method was developed for the simultaneous determination of 6 neonicotinoid insecticides and 3 organophosphorus insecticides including imidacloprid, acetamiprid, thiamethoxam, clothianidin, thiacloprid, dinotefuran, dimethoate, DDVP and chlorpyrifos in honey. The residues were extracted from the samples with acetonitrile and cleaned up with dispersive method on PSA, then detected by ultra liquid chromatography-mass spectrometry under multiple reaction monitoring mode, and quantified by matrix-match standard solution. The results showed the method had good linearity (R≥0.994) from 5-800 μg·L-1. Average fortified recoveries in samples were in the range of 80.4%-107.5% at three fortified levels from 0.005-0.200 mg·kg-1, with relative standard deviations of 1.2%-6.8% (n=5). The limits of detection (LOD) of these 9 insecticides were in the range of 0.1-1.5 μg·kg-1, while limits of quantification (LOQ) were in the range of 0.3-4.5 μg·kg-1. The method is rapid and simple with high sensitivity and good reproducibility, and suitable for determination of different insecticides in honey.
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  • 收稿日期:  2016-03-31
  • 刊出日期:  2016-09-15
李菊颖, 何健, 吴文铸, 孔德洋, 单正军, 陈全博. 蜂蜜中9种杀虫剂的UPLC-MS/MS检测方法[J]. 环境化学, 2016, 35(9): 1921-1927. doi: 10.7524/j.issn.0254-6108.2016.09.2016033101
引用本文: 李菊颖, 何健, 吴文铸, 孔德洋, 单正军, 陈全博. 蜂蜜中9种杀虫剂的UPLC-MS/MS检测方法[J]. 环境化学, 2016, 35(9): 1921-1927. doi: 10.7524/j.issn.0254-6108.2016.09.2016033101
shu
LI Juying, HE Jian, WU Wenzhu, KONG Deyang, SHAN Zhengjun, CHEN Quanbo. UPLC-MS/MS detection of 9 insecticides in honey[J]. Environmental Chemistry, 2016, 35(9): 1921-1927. doi: 10.7524/j.issn.0254-6108.2016.09.2016033101
Citation: LI Juying, HE Jian, WU Wenzhu, KONG Deyang, SHAN Zhengjun, CHEN Quanbo. UPLC-MS/MS detection of 9 insecticides in honey[J]. Environmental Chemistry, 2016, 35(9): 1921-1927. doi: 10.7524/j.issn.0254-6108.2016.09.2016033101
shu

蜂蜜中9种杀虫剂的UPLC-MS/MS检测方法

  • 1. 环境保护部南京环境科学研究所国家环境保护农药环境评价与污染控制重点实验室, 南京, 210042
  • 收稿日期:  2016-03-31
基金项目:

中央级公益性科研院所基本科研业务专项（农药生态影响再评估技术研究2014-002），2013年环保公益行业项目资助项目（2013467026）资助.

摘要: 针对吡虫啉、啶虫脒、噻虫嗪、噻虫胺、噻虫啉、呋虫胺等6种新烟碱类和乐果、敌敌畏、毒死蜱等3种有机磷类杀虫剂建立了蜂蜜中分散固相萃取法-超高效液相色谱-串联质谱的残留分析方法.前处理方法利用乙腈为提取剂，N-丙基乙二胺（PSA）为分散净化剂的QuEChERS方法，并利用超高效液相色谱-串联质谱在多反应离子监测模式（MRM）下进行检测，外标法定量.结果表明，9种杀虫剂在5-800 μg·L-1浓度范围内均具有良好的线性关系（R≥0.994）；在0.005-0.200 mg·kg-1添加，水平范围内平均回收率在80.4%-107.5%之间，相对标准偏差在1.2%-6.8%之间；方法检出限（LOD）在0.1-1.5 μg·kg-1范围内；定量限（LOQ）在0.3-4.5 μg·kg-1范围内.该方法分析速度快、灵敏度高、重现性好，适用于蜂蜜中多种农药残留的快速检测和确证.

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