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    全自动凝胶渗透色谱法净化-气相色谱-串联质谱法测定茄果类蔬菜中7种有机磷类杀虫剂残留量

    Determination of 7 Organophosphorus Pesticide Residues in Solanaceous Vegetables by GC-MS/MS after Purification with Automatic GPC

    • 摘要: 将茄果类蔬菜样品用乙腈萃取后,采用全自动凝胶渗透色谱法(GPC)净化-气相色谱-串联质谱法(GC-MS/MS)测定茄果类蔬菜中7种有机磷类杀虫剂(抑菌灵、毒死蜱、氟菌唑、百菌清、噻菌灵、敌菌灵和戊菌唑)残留量。优化的GPC条件为:体积比1:4的丙酮-环己烷混合溶液为洗脱剂,流量为5 mL·min-1,洗脱时间为8 min,收集时间为6 min;优化的测定条件为:HP-5MS型色谱柱为分离柱,选择电子轰击离子(EI)源和多反应监测(MRM)模式,以环氧七氯为内标物。结果显示:7种有机磷类农药工作曲线的线性范围均为0.05~5.0 mg·L-1,检出限(3S/N)为0.002 2~0.004 5 mg·kg-1。按标准加入法进行回收试验,回收率为94.2%~103%,测定值的相对标准偏差(n=6)均小于5.0%。

       

      Abstract: The sample of solanaceous vegetables was extracted with acetonitrile, and the residual contents of 7 organophosphorus pesticides (i.e., dichlofluanid, chlorphrifos, triflumizole, chlorothalonil, thiabendazole, anilazine, and penconazole) in the purified solution were determined by GC-MS/MS after purification by Autonatic GPC. The optimized conditions of GPC were found:the mixture of acetone and cyclohexane with the volume ratio of 1:4 used as eluent, the flow rate of 5 mL·min-1, the elution time of 8 min, and the collection time of 6 min. The optimized conditions of determined conditions were found:HP-5MS chromatographic column used as separated column, EI and MRM mode adopted in MS/MS analysis, heptachlor epoxide used as internal standard. As found by results, linearity ranges of the standard curves of 7 organophosphorus pesticides were within 0.05-5.0 mg·L-1, with detection limits (3S/N) in the range of 0.002 2-0.004 5 mg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 94.2%-103%, with RSDs (n=6) of the determined values all less than 5.0%.

       

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