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目的:建立蔬菜中49种农药残留量的分散固相萃取-气相色谱-串联质谱(QuEChERS-GC-MS/MS)快速分析方法。方法:样品用乙酸乙酯匀浆提取后,经分散固相萃取法净化,采用气相色谱-串联质谱法用选择反应监测模式SRM进行测定,内标法定量。结果:在0.01 mg/L～10.0 mg/L范围内各农药线性相关系数均大于0.99,分别在菜心、青瓜和土豆中添加浓度水平为0.01 mg/kg和0.02 mg/kg的混标,平均回收率为70.8%～122.5%,方法的相对标准偏差为0.7%～7.8%(n=6)。所有农药的方法定量限均小于10μg/kg。结论:该法前处理简单快速、灵敏、准确,具有良好的回收率和稳定性,较好的解决了样品本底成分复杂的基质干扰,适用于蔬菜中多种农药残留的测定。
OBJECTIVE: To establish a rapid analytical method of dispersive solid phase extraction-gas chromatography-tandem mass spectrometry (QuEChERS-GC-MS / MS) for 49 pesticide residues in vegetables. Methods: The samples were extracted with ethyl acetate and purified by dispersive solid-phase extraction. Gas chromatography-tandem mass spectrometry (LC-MS / MS) was used to determine SRM. Internal standard method was used for quantification. Results: The linear correlation coefficient of each pesticide was more than 0.99 in the range of 0.01 mg / L to 10.0 mg / L, and the mixed standard of 0.01 mg / kg and 0.02 mg / kg was added to cabbage, cucumber and potatoes respectively. The average recoveries ranged from 70.8% to 122.5% with relative standard deviations of 0.7% to 7.8% (n = 6). The limit of quantification for all pesticides is less than 10 μg / kg. Conclusion: The pretreatment method is simple, rapid, sensitive and accurate, and has good recovery and stability. It can solve the complex matrix interference in the background of samples and is suitable for the determination of pesticide residues in vegetables.