李文卓, 钱圆, MATSUMOTO Haruna, 刘晓玉, 秦丽, 王蒙岑, 朱国念. 气相色谱-串联质谱检测蔬菜中氟吡菌酰胺及其代谢物残留[J]. 农药学学报, 2016, 18(6): 759-764. DOI: 10.16801/j.issn.1008-7303.2016.0107
    引用本文: 李文卓, 钱圆, MATSUMOTO Haruna, 刘晓玉, 秦丽, 王蒙岑, 朱国念. 气相色谱-串联质谱检测蔬菜中氟吡菌酰胺及其代谢物残留[J]. 农药学学报, 2016, 18(6): 759-764. DOI: 10.16801/j.issn.1008-7303.2016.0107
    LI Wenzhuo, QIAN Yuan, MATSUMOTO Haruna, LIU Xiaoyu, QIN Li, WANG Mengcen, ZHU Guonian. Simultaneous determination of fluopyram and its metabolite in vegetables using gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2016, 18(6): 759-764. DOI: 10.16801/j.issn.1008-7303.2016.0107
    Citation: LI Wenzhuo, QIAN Yuan, MATSUMOTO Haruna, LIU Xiaoyu, QIN Li, WANG Mengcen, ZHU Guonian. Simultaneous determination of fluopyram and its metabolite in vegetables using gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2016, 18(6): 759-764. DOI: 10.16801/j.issn.1008-7303.2016.0107

    气相色谱-串联质谱检测蔬菜中氟吡菌酰胺及其代谢物残留

    Simultaneous determination of fluopyram and its metabolite in vegetables using gas chromatography-tandem mass spectrometry

    • 摘要: 采用气相色谱-串联质谱(GC-MS/MS)技术建立了同时检测7种类型蔬菜中氟吡菌酰胺及其代谢物残留的分析方法。样品采用乙腈提取,无水硫酸镁和氯化钠盐析后,经分散固相萃取(PSA)净化,GC-MS/MS检测。结果表明:在0.01、0.1和1 mg/kg 3个添加水平下,氟吡菌酰胺及其代谢物2-(三氟甲基)苯甲酰胺(BZM)的平均回收率在80%~108%之间,相对标准偏差(RSD)在1.5%~8.4%之间。氟吡菌酰胺及其代谢物在7种蔬菜中的检出限(LOD)(S/N=3)分别为2.17~3.13 μg/kg和1.22~2.04 μg/kg,两者的定量限(LOQ)均为0.01 mg/kg。该方法操作简便、稳定和快速,可以满足大部分蔬菜中氟吡菌酰胺及其代谢物的定性与定量分析要求。

       

      Abstract: A method was developed for simultaneous determination of fluopyram and its metabolite residues in vegetables by gas chromatography-tandem mass spectrometry (GC-MS/MS). Samples were extracted with acetonitrile, and salted-out by magnesium sulfate and sodium chloride. After clean up with PSA, the analyte was subjected to determination using GC-MS/MS. The results showed that the average recoveries varied from 80% to 108% at the spiked concentrations of 0.01, 0.1 and 1 mg/kg, with the relative standard deviation (RSD) varied from 1.5% to 8.4%. The limits of detection (LOD, S/N=3) varied from 2.17 μg/kg to 3.13 μg/kg for fluopyram in different vegetable samples, while the LOD of fluopyram metabolite varied from 1.22 μg/kg to 2.04 μg/kg. For both fluopyram and its metabolite, the limit of quantification (LOQ) (based on the recovery test) was 0.01 mg/kg. Hence, the method developed in this work is convenient, rapid, reliable, and, more importantly, applicable for qualitative and quantitative analyses of residues of fluopyram and its metabolite in the majority of vegetables.

       

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