郑坤明. QuEChERS-气相色谱-串联质谱法测定中药材水蛭中73种农药残留[J]. 农药学学报, 2022, 24(3): 601-609. DOI: 10.16801/j.issn.1008-7303.2021.0182
    引用本文: 郑坤明. QuEChERS-气相色谱-串联质谱法测定中药材水蛭中73种农药残留[J]. 农药学学报, 2022, 24(3): 601-609. DOI: 10.16801/j.issn.1008-7303.2021.0182
    ZHENG Kunming. Determination of 73 pesticides in traditional Chinese medicine Hirudo by QuEChERS-gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(3): 601-609. DOI: 10.16801/j.issn.1008-7303.2021.0182
    Citation: ZHENG Kunming. Determination of 73 pesticides in traditional Chinese medicine Hirudo by QuEChERS-gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(3): 601-609. DOI: 10.16801/j.issn.1008-7303.2021.0182

    QuEChERS-气相色谱-串联质谱法测定中药材水蛭中73种农药残留

    Determination of 73 pesticides in traditional Chinese medicine Hirudo by QuEChERS-gas chromatography-tandem mass spectrometry

    • 摘要: 建立了中药材水蛭中73种农药的QuEChERS-气相色谱-串联质谱(GC-MS/MS)检测方法。样品用水浸泡并经V(乙酸) : V(乙腈) = 1 : 99和1.5 g乙酸钠溶液作为缓冲体系提取,采用优化的净化剂150 mg乙二胺-N-丙基甲硅烷(PSA)和150 mg十八烷基键合硅胶(C18)组合净化,经HP-5 MS色谱柱分离,在动态多反应监测模式下测定。结果表明:在优化的条件下,10.0~500 μg/L范围内,73种农药在水蛭中的峰面积与其质量浓度间呈良好的线性关系(r > 0.99)。在0.02、0.04和0.2 mg/kg 3个添加水平下,73种农药在水蛭中的回收率为71%~117%,相对标准偏差(RSD)(n = 6)为1.1%~12% (n = 6),定量限(LOQ)为0.02 mg/kg,检出限为0.001~0.008 mg/kg。本方法简捷、灵敏、稳定,可以满足实际检测需求。

       

      Abstract: An analytical method for the simultaneous determination of 73 pesticides in Hirudo using gas chromatography-tandem mass spectrometry(GC-MS/MS) and QuEChERS procedure was developed. After being soaked in water, the samples were extracted with acidic acetonitrile and cleaned up by a mixture of sorbents (150 mg PSA and 150 mg C18). In order to obtain the optimum recovery rate of pesticide analysis, the amounts of the adsorbents were investigated. The analytes were separated by a HP-5 MS column connected to an electron impact ion source(EI) with dynamic multi-reaction monitoring MS mode. Under the optimized conditions, the results showed that the 73 pesticides had good linearity within the range of 10.0-500 μg/L, with correlation coefficients(r) higher than 0.99. The average recoveries ranged from 71%-117%, and the relative standard deviation(RSD) was 1.1%-12% (n=6) at three spiking levels (0.02, 0.04 and 0.2 mg/kg). The LOQs were 0.02 mg/kg and LODs were 0.001-0.008 mg/kg. The method is simple, sensitive, reliable, and can meet the requirements of practical detection for pesticides.

       

    /

    返回文章
    返回