在线凝胶渗透色谱-气相色谱质谱联用仪测定药食同源样品中30种农药残留

Determination of 30 kinds of pesticide residues in homologous samples of medicines and foods by online gel permeation chromatography-gas chromatography-mass spectrometry

目的建立药食同源食品中多种农药残留检测的在线凝胶渗透色谱-气相色谱-质谱联用法(gel permeation chromatography-gas chromatography-mass spectrometry, GPC-GC-MS)。方法本研究采用3种不同净化方式对药食同源样品进行前处理,利用在线凝胶渗透色谱-气相色谱质谱联用仪测定样品中30种农药残留。结果结果表明30种农药在0.01~0.2μg/mL浓度范围内线性关系良好,检出限为0.01 mg/kg,药食同源样品3个水平添加回收为69.1%~88.8%,相对标准偏差为3.3%~19.4%。结论3种方法中QuEChERS法灵敏度高,准确性好,可用于药食同源样品中多种农药残留的同时测定。

Objective To establish a method for determination of pesticide residues in homologous samples of medicines and foods by gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS). Methods Three different purification methods were used for pretreatment of homologous samples of medicines and foods. Thirty kinds of pesticide residues in the samples were determined by GPC-GC-MS. Results The results showed that 30 kinds of pesticides had good linear relationships in the range of 0.01-0.2 μg/mL, the limits of detection were 0.01 mg/kg, and the recoveries at 3 spiked levels of the three added levels of the homologous samples of medicines and foods samples were 69.1%-88.8%, with the relative standard deviations of 3.3%-19.4%. Conclusion Among the three methods, QuEChERS method has high sensitivity and accuracy, which can be used for simultaneous determination of multiple pesticide residues in the homologous samples of medicines and foods.