刘佳悦, 徐军, 张云慧, 王丽川, 董丰收, 吴小虎, 潘兴鲁, 郑永权. 噻虫嗪及其代谢物噻虫胺在麦叶和麦穗中的痕量检测方法及其应用[J]. 农药学学报, 2022, 24(1): 133-141. DOI: 10.16801/j.issn.1008-7303.2021.0153
    引用本文: 刘佳悦, 徐军, 张云慧, 王丽川, 董丰收, 吴小虎, 潘兴鲁, 郑永权. 噻虫嗪及其代谢物噻虫胺在麦叶和麦穗中的痕量检测方法及其应用[J]. 农药学学报, 2022, 24(1): 133-141. DOI: 10.16801/j.issn.1008-7303.2021.0153
    LIU Jiayue, XU Jun, ZHANG Yunhui, WANG Lichuan, DONG Fengshou, WU Xiaohu, PAN Xinglu, ZHENG Yongquan. Trace determination of thiamethoxam and clothianidin in wheat leaves and wheat ears and its application[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 133-141. DOI: 10.16801/j.issn.1008-7303.2021.0153
    Citation: LIU Jiayue, XU Jun, ZHANG Yunhui, WANG Lichuan, DONG Fengshou, WU Xiaohu, PAN Xinglu, ZHENG Yongquan. Trace determination of thiamethoxam and clothianidin in wheat leaves and wheat ears and its application[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 133-141. DOI: 10.16801/j.issn.1008-7303.2021.0153

    噻虫嗪及其代谢物噻虫胺在麦叶和麦穗中的痕量检测方法及其应用

    Trace determination of thiamethoxam and clothianidin in wheat leaves and wheat ears and its application

    • 摘要: 建立了超高效液相色谱-串联质谱 (UPLC-MS/MS)测定麦叶和麦穗中噻虫嗪及其代谢物噻虫胺残留的痕量、快速检测方法。麦叶或麦穗中噻虫嗪及其代谢物噻虫胺用乙腈提取,NH2/Carb固相萃取柱净化,内标法定量。结果表明:噻虫嗪和噻虫胺在0.001 ~ 0.5 mg/L范围内线性关系良好,相关系数r大于0.99;噻虫嗪和噻虫胺在0.001、0.01、0.1和1 mg/kg 4个添加水平下,在麦叶和麦穗中的平均回收率为83% ~ 118%之间,相对标准偏差 (RSD)在1.6% ~ 13.0% 之间。定量限可达到0.001 mg/kg。运用该检测方法测定了采用植保无人机喷施 25%噻虫嗪水分散粒剂 (有效成分37.5 g/hm2) 后的麦叶和麦穗样品,发现施药后2 h麦叶和麦穗中噻虫嗪的残留量分别为4.24和1.34 mg/kg,施药后14 d麦叶中噻虫嗪和噻虫胺的残留量分别为0.097和0.079 mg/kg,麦穗中的分别为0.031和0.046 mg/kg。该方法可满足小麦全生育期检测需求,运用该方法可研究噻虫嗪及噻虫胺在小麦植株内的传导分布特点及残留代谢过程。

       

      Abstract: A rapid and trace analytical method was established for the determination of thiamethoxam and its metabolite clothianidin in wheat leaves and wheat ears using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Wheat leaves and wheat ears were extracted with acetonitrile and cleaned up with NH2/Carb solid phase extraction column to remove impurities such as chlorophyll and starch. The internal standard method was used for quantitation. The results showed that the linearity of thiamethoxam and clothianidin was good in the range of 0.001-0.5 mg/L, and the correlation coefficient was greater than 0.99. After internal standard correction, the recoveries of thiamethoxam and clothianidin in wheat leaves and wheat ears were in the range from 83.4% to 117.9% at 4 levels of 0.001, 0.01, 0.1 and 1 mg/kg, and the relative standard deviations were in the range of 1.6% to 13.0%. The limit of quantitation was 0.001 mg/kg. This method was used to determine the wheat leaves and wheat ears field samples after the wheat crops were sprayed with thiamethoxam 250 WG by unmanned aerial vehicle (UAV). The concentrations of thiamethoxam in wheat leaves and wheat ears were 4.24 and 1.34 mg/kg, respectively, at 2 h after application. On the 14th day after application, the concentrations of thiamethoxam and clothianidin were 0.097 and 0.079 mg/kg in wheat leaves, and were 0.031 and 0.046 mg/kg in wheat ears, respectively. This method can meet the detection requirements of wheat during the whole growth period, and it can also be used to study the conduction and distribution characteristics and residual metabolism of thiamethoxam and clothianidin in wheat plants.

       

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