毛细管气相色谱法测定金银花中敌敌畏、甲基对硫磷和马拉硫磷的残留量

目的：建立测定金银花中敌敌畏、甲基对硫磷和马拉硫磷残留量的毛细管气相色谱分析方法。方法：样品以微波提取的方法进行处理。以FPD为检测器,色谱柱为HP-5石英毛细管柱（25m×0.32mm,0.17μm）,载气为高纯氮气,流速20ml/min;氢气流速45ml/min;空气流速450ml/min;程序升温：初始温度为120℃,最终温度为230℃,升温速率10℃/min。进样口温度250℃,检测器温度260℃。采用无分流进样方式。结果：敌敌畏、甲基对硫磷和马拉硫磷的测定浓度在0.25￣3.00μg/ml时,浓度与峰面积呈线性关系。当信噪比为2时,敌敌畏的最低检出量为0.3ng,甲基对硫磷的最低检出量为0.15ng,马拉硫磷的最低检出量为0.2ng。敌敌畏的平均回收率为88.7%,RSD为2.1%;甲基对硫磷平均回收率为89.7%,RSD为1.7%,马拉硫磷平均回收率为90.6%,RSD为1.1%。结论：该方法操作简便、准确、可靠,可用于金银花中敌敌畏、甲基对硫磷和马拉硫磷残留量的测定。

Determination of the residue of dichlorovos,methyl parathion and malathion in Flos Lonicerae by capillary gas chromatography

Objective： To develop a capillary gas chromatography method for determining the residue of dichlorovos, methyl parathion and malathion in Flos Lonicerae. Methods： The samples were treated with microwave extraction and separated by HP-5 capillary column （25 m×0.32 mm, 0.17μm） with FPD. Highly pure nitrogen was used as carrier gas,and the flow rate was 20 ml/min. Hydrogen flow rate was 45 ml/min, and air flow rate was 450 ml/min. Temperature programming from 120℃ to 230℃ was 10℃/min;injector temperature was 250℃; detector temperature was 260℃. The mode of injection was splitless. Results： The linear range of dichlorovos, methyl parathion and malathion was 0.25 -3.00 μg/ml. When the S/N was 2, the detection limit of dichlorovos was 0.3 ng, methyl parathion was 0.15 ng,and malathion was 0.2 ng. The average recovery of dichlorovos was 88.7% with RSD of 2.1%, methyl parathion was 89.7% with RSD of 1.7% and malathion was 90.6% with RSD of 1.1%.Conclusion： The method is easy, accurate and suitable for determining the residue of dichlorovos, methyl parathion and malathion in Flos Lonicerae.