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牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发

叶倩 朱富伟 王刚 廖林瀚 唐雪妹

叶倩, 朱富伟, 王刚, 廖林瀚, 唐雪妹. 牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发[J]. 农药学学报, 2022, 24(2): 404-410. doi: 10.16801/j.issn.1008-7303.2021.0170
引用本文: 叶倩, 朱富伟, 王刚, 廖林瀚, 唐雪妹. 牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发[J]. 农药学学报, 2022, 24(2): 404-410. doi: 10.16801/j.issn.1008-7303.2021.0170
YE Qian, ZHU Fuwei, WANG Gang, LIAO Linhan, TANG Xuemei. Development of gas chromatography-tandem mass spectrometry detection method for 14 herbicides residues in milk[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 404-410. doi: 10.16801/j.issn.1008-7303.2021.0170
Citation: YE Qian, ZHU Fuwei, WANG Gang, LIAO Linhan, TANG Xuemei. Development of gas chromatography-tandem mass spectrometry detection method for 14 herbicides residues in milk[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 404-410. doi: 10.16801/j.issn.1008-7303.2021.0170

牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发

doi: 10.16801/j.issn.1008-7303.2021.0170
基金项目: 国家重点研发计划(2019YFC1605204);广东省基础与应用基础研究基金项目(2020A1515010620);广东省农业科学院科技创新战略专项资金(高水平农科院建设).
详细信息
    作者简介:

    叶倩,yeqian.liao@foxmail.com

    通讯作者:

    唐雪妹,xuemeitang@gdaas.cn.

  • 中图分类号: O657.63;TS207

Development of gas chromatography-tandem mass spectrometry detection method for 14 herbicides residues in milk

Funds: National Key Research and Development Program of China (2019YFC1605204), Natural Science Foundation of Guangdong Province (2020A1515010620), Special Fund for Science and Technology Innovation Strategy (Construction of High-Levelacademy of Agricultural Sciences of Guangdong Province).
  • 摘要: 建立了同时快速检测牛奶中14种除草剂残留的气相色谱-串联质谱(GC-MS/MS)分析方法。样品采用乙腈提取,无水硫酸镁和无水乙酸钠净化,过0.22 μm有机相滤膜后,目标物采用气相色谱-串联质谱(EI离子源)、多反应监测模式(MRM)检测。结果表明:在0.005~1 mg/L范围内,14种目标除草剂的质量浓度与其相应峰面积间呈良好的线性关系,决定系数(R2)均大于0.9902。在0.01、0.05和0.5 mg/kg 3个添加水平下,14种除草剂的平均回收率为76%~113%,相对标准偏差(RSD)为1.2%~8.6% (n=6)。14种除草剂在牛奶中的定量限(LOQ)均为0.01 mg/kg。该方法准确、灵敏、操作步骤简单,适用于同时快速测定牛奶中14种除草剂的残留量。
  • 图  1  牛奶基质中14种除草剂的多反应监测色谱图

    Figure  1.  Chromatography of 14 herbicides in milk matrix by MRM mode

    图  2  不同提取溶剂对14种除草剂的提取效果

    Figure  2.  Extraction effects of 14 herbicides by different extraction solvents

    图  3  乙腈用量对14种除草剂提取效果的影响

    Figure  3.  Extraction effects of 14 herbicides by different volumes of acetonitrile

    图  4  不同净化方式对14种除草剂的净化效果

    Figure  4.  Purification effect of 14 herbicides by different adsorbents

    表  1  14种除草剂的CAS号、保留时间、定量和定性离子对及碰撞能量

    Table  1.   The CAS No., retention time, optimized ion pairs and collision energy for the 14 herbicides

    除草剂
    Herbicide
    CAS 号
    CAS No.
    保留时间
    Retention time/min
    定量及定性离子对,m/z
    Q1/Q3
    碰撞电压
    CE/V
    氯苯胺灵 chlorpropham 101-21-3 8.65 153/125.1*, 153/90, 127/65.1 10, 25, 25
    氟乐灵 trifluralin 1582-09-8 9.06 305.9/264*, 264/160.1, 264/206.2 5, 15, 5
    莠去津 atrazine 1912-24-9 10.64 214.9/58.1*, 214.9/200.2, 200/122.1 10, 5, 5
    二甲吩草胺 dimethenamid 87674-68-8 14.27 230/154.1*, 154.1/111.1, 232/154.1 10, 10, 10
    乙草胺 acetochlor 34256-82-1 14.71 174/146.1*, 146/131.1, 222.9/132.2 10, 10, 20
    甲草胺 alachlor 15972-60-8 15.44 188.1/160.2*, 160/132.1, 188.1/132.1 10, 10, 15
    莠灭净 ametryn 834-12-8 15.66 227/58.1*, 185/170, 227/170.1 10, 5, 10
    扑草净 prometryn 7287-19-6 16.02 226/184.2*, 199/184.1, 241/184.2 10, 5, 10
    异丙甲草胺 metolachlor 51218-45-2 17.73 238/162.2*, 162.2/133.2, 240/162.2 10, 15, 10
    二甲戊灵 pendimethalin 40487-42-1 19.09 251.8/162.2*, 251.8/161.1, 161.9/161.1 10, 15, 10
    丁草胺 butachlor 23184-66-9 20.08 176.1/147.1*, 188.1/160.2, 160.1/132.1 10, 10, 10
    敌草胺 napropamide 15299-99-7 20.18 128/72.1*, 128/100.1, 271/72.1 5, 10, 15
    丙草胺 pretilachlor 51218-49-6 20.45 162.1/147.2*, 162.1/132.2, 262/202.2 10, 20, 5
    除草醚 nitrofen 1836-75-5 20.85 202/139.1*, 282.9/253, 282.9/202 20, 10, 10
    注:*定量离子对。Note: *indicate quantitative ion.
    下载: 导出CSV
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  • 收稿日期:  2021-06-24
  • 录用日期:  2021-09-12
  • 网络出版日期:  2021-11-03
  • 刊出日期:  2022-04-01

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