陈敏, 刘茜, 杨晓凤. 气相色谱-串联质谱法测定干辣椒中50种农药残留[J]. 农药学学报, 2021, 23(4): 771-780. DOI: 10.16801/j.issn.1008-7303.2021.0078
    引用本文: 陈敏, 刘茜, 杨晓凤. 气相色谱-串联质谱法测定干辣椒中50种农药残留[J]. 农药学学报, 2021, 23(4): 771-780. DOI: 10.16801/j.issn.1008-7303.2021.0078
    CHEN Min, LIU Qian, YANG Xiaofeng. Determination of 50 pesticide residues in dry chilli by gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(4): 771-780. DOI: 10.16801/j.issn.1008-7303.2021.0078
    Citation: CHEN Min, LIU Qian, YANG Xiaofeng. Determination of 50 pesticide residues in dry chilli by gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(4): 771-780. DOI: 10.16801/j.issn.1008-7303.2021.0078

    气相色谱-串联质谱法测定干辣椒中50种农药残留

    Determination of 50 pesticide residues in dry chilli by gas chromatography-tandem mass spectrometry

    • 摘要: 建立了固相萃取结合气相色谱-串联质谱 (GC-MS/MS) 测定干辣椒中敌草腈、氟唑菌酰胺、氟吡菌胺、苯菌酮等50种农药残留量的方法。样品加水浸泡后用乙腈提取,加入氯化钠盐析并离心,取上清液经复合氨基柱净化,用乙酸乙酯定容至1.0 mL后,采用气相色谱-串联质谱法在多反应监测 (MRM) 模式下检测,基质匹配标准曲线外标法定量。结果表明:50种农药中,有46种农药在0.005~0.5 mg/L质量浓度范围内线性关系良好,R2 ≥ 0.99;定量限 (LOQ) 范围为0.01~0.1 mg/kg;在0.01、0.1和1.0 mg/kg 3个添加水平下46种农药在干辣椒中的平均回收率在72%~120%之间,相对标准偏差 (RSD) 在0.7%~17%之间。该方法简单、快速、高效,且灵敏度、准确度、精密度均可满足日常检测需求,适用于干辣椒样品中多农药残留的同时检测。

       

      Abstract: A method for the determination of 50 pesticide residues such as dichlobenil, fluxapyroxad, fluopicolide, metrafenone, etc, in dry chilli was established using solid phase extraction (SPE) combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). After being soaked in water, the samples were extracted with acetonitrile, salted out with sodium chloride, and then centrifuged. The supernatant was cleaned-up by SPE column of CARB/NH2, then dissolved and diluted to 1.0 mL with ethyl acetate. The targeted compounds were detected by GC-MS/MS and then quantified by the matrix-matched external standard calibration method. The results showed that among the 50 pesticides, 46 analytes displayed good linearity in the range of 0.005-0.5 mg/L, with determination coefficient (R2) ≥ 0.99. The limits of quantitation (LOQ) ranged from 0.01 to 0.1 mg/kg. The average recoveries for the 46 pesticides at spiked levels of 0.01, 0.1, 1.0 mg/kg in dry chilli were in the range of 72%-120%, and the relative standard deviations (RSD) were between 0.7% and 17%. The method is simple, rapid, highly efficient, and the sensitivity, accuracy, and precision meet the daily routine testing requirements. It is suitable for the simultaneous detection of multiple pesticide residues in dry chilli samples.

       

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