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    潘苗, 于卫松, 鲁世军, 曹建敏, 孙惠青. GC-MS/MS测定烟草上氟唑菌酰羟胺残留[J]. 中国烟草科学, 2023, 44(6): 53-58. DOI: 10.13496/j.issn.1007-5119.2023.06.008
    引用本文: 潘苗, 于卫松, 鲁世军, 曹建敏, 孙惠青. GC-MS/MS测定烟草上氟唑菌酰羟胺残留[J]. 中国烟草科学, 2023, 44(6): 53-58. DOI: 10.13496/j.issn.1007-5119.2023.06.008
    PAN Miao, YU Weisong, LU Shijun, CAO Jianmin, SUN Huiqing. GC-MS/MS Determination of Pydiflumetofen Residues in Tobacco[J]. CHINESE TOBACCO SCIENCE, 2023, 44(6): 53-58. DOI: 10.13496/j.issn.1007-5119.2023.06.008
    Citation: PAN Miao, YU Weisong, LU Shijun, CAO Jianmin, SUN Huiqing. GC-MS/MS Determination of Pydiflumetofen Residues in Tobacco[J]. CHINESE TOBACCO SCIENCE, 2023, 44(6): 53-58. DOI: 10.13496/j.issn.1007-5119.2023.06.008

    GC-MS/MS测定烟草上氟唑菌酰羟胺残留

    GC-MS/MS Determination of Pydiflumetofen Residues in Tobacco

    • 摘要: 为填补行业领域空白,本研究建立了气相色谱-串联质谱多反应监测模式(MRM)测定烟草上氟唑菌酰羟胺残留量的检测方法,并通过田间试验分析了氟唑菌酰羟胺在烟草上的消解动态。结果表明,该方法在0.001~0.5 mg/L质量浓度范围内进样浓度和响应峰面积之间的线性良好,决定系数R2=0.999 5;测定RSD为4.57%,测定定量限0.012 mg/kg。在0.012、0.12和0.5 mg/kg 3个添加水平下,平均回收率在92.6%~101.7%之间,RSD在2.6%~4.5%范围内。氟唑菌酰羟胺在四川、山东两地烟草上的消解趋势符合一级动力学方程,取样间隔5 d和35 d时烟草上氟唑菌酰羟胺的消解率分别超过50%和90%,理论半衰期在5.73~9.12 d之间。国内和CORESTA暂未制定氟唑菌酰羟胺在烟草上的MRL和检测方法标准,研究结果可为其限量标准、检测标准的制定提供数据和方法参考。

       

      Abstract: In order to fill the gap in the field, a gas chromatography-tandem mass spectrometry multi-reaction monitoring mode (MRM) was established for the determination of pydiflumetofen residue in tobacco, and the digestion resolution dynamics of pydiflumetofen in tobacco were analyzed through field experiments. The results show that the method has good linearity in the mass concentration range of 0.001~0.5 mg/L, and the correlation coefficient R2=0.999 5; RSD was 4.57% when repeated determination of the same test sample, and the limit of quantification was 0.012 mg/kg. At 0.012, 0.12 and 0.5 mg/kg supplemental levels, the average recovery rate ranged from 92.6% to 101.7%, and RSD ranged from 2.6% to 4.5%. The digestion trend of pydiflumetofen in tobacco in Sichuan and Shandong was in line with the first-order kinetic equation. The digestion rate of pydiflumetofen in tobacco was more than 50% and 90% at sampling interval of 5 d and 35 d, the theoretical half-life of pydiflumetofen in tobacco was between 5.73 d and 9.12 d. MRL is not established in China or by CORESTA for detection method standards for pydiflumetofen in tobacco, and the research results can provide data and method reference for the formulation of limit standards and detection standards.

       

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