杨金川, 张建, 白雪梅. QuEChERS-气相色谱-质谱法测定粮谷中氰烯菌酯残留[J]. 农药学学报, 2020, 22(6): 1099-1103. DOI: 10.16801/j.issn.1008-7303.2020.0150
    引用本文: 杨金川, 张建, 白雪梅. QuEChERS-气相色谱-质谱法测定粮谷中氰烯菌酯残留[J]. 农药学学报, 2020, 22(6): 1099-1103. DOI: 10.16801/j.issn.1008-7303.2020.0150
    YANG Jinchuan, ZHANG Jian, BAI Xuemei. Determination of phenamacril in cereals by QuEChERS-gas chromatography-mass spectrometry[J]. Chinese Journal of Pesticide Science, 2020, 22(6): 1099-1103. DOI: 10.16801/j.issn.1008-7303.2020.0150
    Citation: YANG Jinchuan, ZHANG Jian, BAI Xuemei. Determination of phenamacril in cereals by QuEChERS-gas chromatography-mass spectrometry[J]. Chinese Journal of Pesticide Science, 2020, 22(6): 1099-1103. DOI: 10.16801/j.issn.1008-7303.2020.0150

    QuEChERS-气相色谱-质谱法测定粮谷中氰烯菌酯残留

    Determination of phenamacril in cereals by QuEChERS-gas chromatography-mass spectrometry

    • 摘要: 建立了一种适用QuEChERS前处理结合气相色谱-质谱 (GC-MS) 技术测定4种粮谷(糙米、小麦、高粱及玉米)中氰烯菌酯残留的方法。样品经乙腈提取、PSA净化和浓缩后,采用GC-MS检测,内标法定量。结果表明:在10~500 μg/L质量浓度范围内,氰烯菌酯峰面积与进样质量浓度间线性关系良好,决定系数 (R2) > 0.9983,定量限 (LOQ) 低于0.005 mg/kg;在添加水平分别为0.005、0.02、0.05及0.1 mg/kg时,该方法的平均回收率在85%~108%之间,相对标准偏差 (RSDs) 为1.1%~10.4%。该方法简便、快速,具有良好的灵敏度和重现性,适用于粮谷中氰烯菌酯的残留量测定。

       

      Abstract: A method was developed for the determination of phenamacril residue in four kinds of cereals (rice, wheat, sorghum, corn) by QuEChERS combined with gas chromatography-mass spectrometry (GC-MS). The samples were extracted with acetonitrile, cleaned-up with PSA, concentrated, and detected by GC-MS using internal standard method. The results showed that the linear relationship of phenamacril in the linear range from 10 to 500 μg/L was good, the linear correlation coefficients (R2) was higher than 0.998 3, with the limit of quantitation (LOQs) lower than 0.005 mg/kg. The average recoveries at four spiking levels (0.005 mg/kg, 0.02 mg/kg, 0.05 mg/kg, 0.1 mg/kg) in cereals ranged from 85% to 108%, and the relative standard deviations (RSDs) were from 1.1% to 10.4%. This method was simple, rapid, sensitive and applicable to the determination of phenamacril in cereals.

       

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