张斌斌, 董丰收, 潘兴鲁, 吴小虎, 徐军, 郑永权. 超高效液相色谱-串联质谱同时检测水稻中3种农药及2种代谢物残留[J]. 农药学学报, 2022, 24(6): 1508-1517. DOI: 10.16801/j.issn.1008-7303.2022.0047
    引用本文: 张斌斌, 董丰收, 潘兴鲁, 吴小虎, 徐军, 郑永权. 超高效液相色谱-串联质谱同时检测水稻中3种农药及2种代谢物残留[J]. 农药学学报, 2022, 24(6): 1508-1517. DOI: 10.16801/j.issn.1008-7303.2022.0047
    ZHANG Binbin, DONG Fengshou, PAN Xinglu, WU Xiaohu, XU Jun, ZHENG Yongquan. Determination of the residues of three pesticides and two metabolites in rice by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(6): 1508-1517. DOI: 10.16801/j.issn.1008-7303.2022.0047
    Citation: ZHANG Binbin, DONG Fengshou, PAN Xinglu, WU Xiaohu, XU Jun, ZHENG Yongquan. Determination of the residues of three pesticides and two metabolites in rice by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(6): 1508-1517. DOI: 10.16801/j.issn.1008-7303.2022.0047

    超高效液相色谱-串联质谱同时检测水稻中3种农药及2种代谢物残留

    Determination of the residues of three pesticides and two metabolites in rice by ultra-high performance liquid chromatography-tandem mass spectrometry

    • 摘要: 建立并优化了基于超高效液相色谱-串联质谱 (UPLC-MS/MS) 同时检测水稻中甲氨基阿维菌素苯甲酸盐、氯虫苯甲酰胺、氟唑菌酰胺及其代谢物M700F008、M700F048的分析方法。稻壳和糙米经0.2%甲酸-乙腈提取后用C18净化,稻秆经1%甲酸-乙腈提取后用N-丙基乙二胺 (PSA) 和石墨化碳黑 (GCB) 净化,流动相为甲醇和0.2%甲酸水溶液,梯度洗脱,采用T3色谱柱进行分离。电喷雾正离子模式 (ESI+) 采集,多反应监测 (MRM),外标法定量。结果表明:5种供试化合物的质量浓度与峰面积间线性关系良好,决定系数均大于0.9955;5种化合物在水稻稻壳、糙米及稻秆3种基质中的平均回收率均在71%~119%之间,相对标准偏差 (RSD) 在1%~11%之间,满足残留分析的要求。在3地供试糙米样品中,甲氨基阿维菌素苯甲酸盐、氯虫苯甲酰胺和氟唑菌酰胺的残留量均低于中国规定的最大残留限量标准。

       

      Abstract: An analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry was established and optimized for simultaneous determination of emamectin benzoate, chlorantraniliprole, fluxapyroxad and its metabolites M700F008 and M700F048 in rice. Rice husk and brown rice were extracted with 0.2% formic acid-acetonitrile and cleaned up with C18, while rice straw was extracted with 1% formic acid-acetonitrile and cleaned up with N-propyl ethylenediamine (PSA) and graphitized carbon black (GCB). T3 chromatographic column was used for separation and the mobile phase was methanol and 0.2% formic acid water. Electrospray ionization in positive ion mode was selected, the detection mode was multi-reaction monitoring, and external standard method was used for quantification. The results showed that there was a good linear relationship between the mass concentration and peak area of the five tested compounds, and the determination coefficient was greater than 0.9955. The average recoveries of the five compounds in rice husk, brown rice and rice straw were in range of 71%-119% with the relative standard deviations (RSD) of 1%-11%, which met the requirements of residue analysis. The residues of emamectin benzoate, chlorantraniliprole and fluxapyroxad in brown rice samples collected from three locations were all lower than MRLs in China.

       

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