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优化的QuEChERS-超高效液相色谱-串联质谱法测定韭菜中31种农药残留

李浩林 李桐桐 董玉英 禾丽菲 李北兴 慕卫

李浩林, 李桐桐, 董玉英, 禾丽菲, 李北兴, 慕卫. 优化的QuEChERS-超高效液相色谱-串联质谱法测定韭菜中31种农药残留[J]. 农药学学报. doi: 10.16801/j.issn.1008-7303.2021.0054
引用本文: 李浩林, 李桐桐, 董玉英, 禾丽菲, 李北兴, 慕卫. 优化的QuEChERS-超高效液相色谱-串联质谱法测定韭菜中31种农药残留[J]. 农药学学报. doi: 10.16801/j.issn.1008-7303.2021.0054
Haolin LI, Tongtong LI, Yuying DONG, Lifei HE, Beixing LI, Wei MU. Determination of 31 pesticide residues in Chinese chives by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science. doi: 10.16801/j.issn.1008-7303.2021.0054
Citation: Haolin LI, Tongtong LI, Yuying DONG, Lifei HE, Beixing LI, Wei MU. Determination of 31 pesticide residues in Chinese chives by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science. doi: 10.16801/j.issn.1008-7303.2021.0054

优化的QuEChERS-超高效液相色谱-串联质谱法测定韭菜中31种农药残留

doi: 10.16801/j.issn.1008-7303.2021.0054
基金项目: 国家自然科学基金 (32072463;32001953)
详细信息
    作者简介:

    李浩林,男,硕士研究生,E-mail:1594568916@qq.com

    通讯作者:

    慕卫,通信作者 (Author for correspondence),女,教授,研究方向为农药残留分析与环境毒理,E-mail:muwei@sdau.edu.cn

  • 中图分类号: S482; TQ450.263; O657.63

Determination of 31 pesticide residues in Chinese chives by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

  • 摘要: 基于超高效液相色谱-串联质谱 (UPLC-MS/MS),建立了同时检测韭菜中31种农药残留的分析方法。韭菜样品经乙腈提取,采用QuEChERS方法净化后,进行UPLC-MS/MS 检测。结果表明:在 0.5~100 μg/L范围内,31种农药的质量浓度与相应的峰面积间呈良好的线性关系,相关系数均大于0.995,定量限 (LOQ) 为10 μg/kg;在0.01、0.1和1 mg/kg 3个添加水平下,31种农药在韭菜中的平均回收率在70%~102%之间,相对标准偏差 (RSD) 均小于11%(n = 5)。该方法快速、简便、可靠、高效,且成本低廉,适用于同时检测韭菜中 31种农药的残留量。
  • 表  1  31种农药在 UPLC-MS/MS 多反应监测模式下的检测条件

    Table  1.   Multiple reaction monitoring conditions for the determination of 31 pesticides using UPLC-MS/MS

    分析物    
    Analyte    
    保留时间
    Retention time/min
    定量和定性离子对
    Quantitative, qualitative ion pair, m/z
    碰撞能
    Collision energy/eV
    灭多威 methomyl 2.09 163.00 > 88.00*, 106.00 10, 10
    异丙威 isoprocarb 3.98 194.10 > 95.10*, 137.10 15, 10
    莠去津 atrazine 3.99 216.10 > 96.00*, 174.00 22, 15
    敌敌畏 dichlorvos 3.59 221.00 > 79.00*, 109.00 34, 22
    克百威 carbofuran 3.57 222.11 > 123.00*, 165.10 20, 10
    乐果 dimethoate 2.82 230.10 > 125.00*, 199.00 10, 20
    扑草净 prometryn 4.35 242.10 > 158.00*, 200.00 22, 16
    噻虫胺 clothianidin 2.62 250.00 > 132.00*, 169.00 15, 10
    吡虫啉 imidacloprid 2.55 256.10 > 175.10*, 209.10 30, 15
    敌百虫 trichlorfon 2.81 257.00 > 79.00*, 109.00 30, 15
    烯啶虫胺 nitenpyram 1.94 271.10 > 125.90*, 224.90 30, 10
    二甲戊灵 pendimethalin 6.39 282.20 > 194.10*, 212.20 17, 10
    异丙甲草胺 s-metolachlor 4.88 284.00 > 176.00*, 252.00 25, 12
    噻虫嗪 thiamethoxam 2.19 292.00 > 132.00*, 211.20 20, 10
    三唑酮 triadimefon 4.55 294.10 > 69.30*, 197.20 20, 15
    仲丁灵 butralin 6.56 296.20 > 222.00*, 240.00 21, 11
    辛硫磷 phoxim 5.31 299.00 > 129.00*, 153.00 13, 7
    克线磷 fenamiphos 4.91 304.10 > 202.10*, 217.10 36, 24
    二嗪农 diazinon 5.22 305.10 > 96.90*, 169.00 25, 22
    戊唑醇 tebuconazole 5.19 308.00 > 70.00*, 125.00 12, 35
    吡丙醚 pyriproxifen 6.18 322.10 > 96.00*, 227.10 15, 10
    噁草灵 oxadiazon 6.13 345.20 > 220.00*, 303.00 18, 12
    毒死蜱 chlorpyrifos 6.31 350.10 > 97.00*, 125.00 34, 14
    甲氰菊酯 fenpropathrin 6.31 349.90 > 97.00*, 198.00 32, 20
    哒螨灵 pyridaben 6.87 365.10 > 147.10*, 309.10 24, 12
    精喹禾灵 quizalofop-p-tefuryl 5.88 373.10 > 271.10*, 299.10 22, 16
    丁硫克百威 carbosulfan 7.22 381.00 > 76.00*, 118.00 34, 22
    醚菊酯 etofenprox 7.37 394.30 > 106.90*, 177.00 43, 15
    氟虫腈 fipronil 4.91 453.90 > 368.10*, 404.25 25, 19
    氟啶脲 chlorfluazuron 6.73 539.80 > 158.00*, 382.90 15, 20
    阿维菌素 abamectin (B1a) 7.05 895.40 > 183.10*, 751.40 54, 40
    注:*表示定量离子。Note: * Represents the quantitative ion pair.
    下载: 导出CSV
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出版历程
  • 收稿日期:  2020-10-02
  • 录用日期:  2020-11-11
  • 网络出版日期:  2021-01-08

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