混合固相萃取柱净化-气相色谱质谱联用法快速测定果蔬中10种农药残留的研究

Rapid determination of 10 pesticides in fruits and vegetables by mixed solid-phase extraction column purification gas chromatography-mass spectrometry

目的:建立果蔬中10种除草剂、杀菌剂、杀虫剂农残的混合固相萃取柱-气相色谱质谱联用分析方法。方法:样品经乙腈提取,盐析,活性炭-氨基混合柱净化,采用气相色谱-质谱测定,基质匹配外标法定量。结果:在0.05μg/ml～2.00μg/ml范围内,相关系数r>0.992,样品在0.05 mg/kg～0.50 mg/kg范围内加标,平均回收率在79.77%～118.33%之间,相对标准偏差(RSD)为3.17%～11.35%,检测限(LOD)在0.001 mg/kg～0.006 mg/kg之间。结论:该方法快速、可操作性强、净化效果较好,可同时满足蔬菜水果中多种农药残留的检测需要。

Objective：To establish a method for determining 10 pesticides in fruits and vegetables by gas chromatography-mass spectrometry（GC-MS） with mixed solid-phase extraction column purification.Methods： Samples were extracted by acetonitrile,purified through Carb-HN2 column after salting out and finally quantified with matrix-matched external standards.Results： The linear range of 10 pesticides was 0.05 μg/ml^2.00 μg/ml（r〉0.992）.Within the adding scope of 0.05 mg/kg^0.5 mg/kg,average recovery rate were 79.77%~118.33%,relative standard deviation（RSD） was 3.17%~11.35%,detection limit of the method was 0.001 mg/kg^0.006 mg/kg.Conclusion： Results show that the method is rapid,applicable,accurate with good purification for determining residual pesticides in fruits and vegetables.