超高效液相色谱-串联质谱法测定蔬菜中7种氨基甲酸酯类农药残留

Determination of Carbamate Residues in Vegetables by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

建立蔬菜中氨基甲酸酯类农药残留的超高效液相色谱-串联质谱联用的确证方法。样品经乙腈提取后,氨基柱净化,采用UPLC-MS/MS正离子模式下选择多反应监测(MRM)扫描测定。7种氨基甲酸酯类农药在5～200μg/L范围内线性关系良好,相关系数为0.9977～0.9999。在0.01～0.10mg/kg添加范围内,回收率范围在72.1%～110.2%之间,相对标准偏差为1.7%～9.4%,方法的最低检出限为0.5～8..0μg/kg(RSN=10)。该方法操作简单、灵敏、准确度高,完全可满足蔬菜中多种氨基甲酸酯类农药残留量的测定及确证工作的需要。

A simultaneous determination method for 7 kinds of carbamate residues in vegetables was developed by ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.The samples was extracted with acetonitrile and cleaned-up by NH2 solid phase extraction（SPE） cartridges.The analytes were quantified by UPLC-MS/MS in a positive ion multiple reaction mode（MRM）.An excellent linear relationship for 7 carbamate residues was observed in the concentration range of 5-200μg/L with the regression coefficients of 0.9977-0.9999.The average recovery rate of 7 carbamate residues in vegetables at the spiked level of 0.01-0.10 mg/kg was in the range of 72.1%-110.2% with relative standard deviation of 1.7%-9.4%.This developed method revealed a detection limit range of 0.5-8.0μg/kg（RSN = 10）.Therefore,this developed method is characteristics of simple operation,high sensitivity and precision,which can meet the requirements for simultaneous determination of carbamate pesticide residues in vegetables for inspection and confirmation.