建立了菊花中25种有机氯农药多残留量的气相色谱-电子捕获检测器分析方法。样品以石油醚-丙酮(体积比1∶1)为提取剂,冰浴超声提取,提取液用浓硫酸净化,采用HP-5与DB1701毛细管色谱柱双柱定性分离,电子捕获检测器(ECD)测定25种有机氯农药的残留量。结果表明:在20、50、100μg/kg 3个添加水平下的回收率分别在69.9%~113.9%、69.4%~100.3%、70.1%~103.1%,相对标准偏差(RSD)分别为2.3%~11.9%、3.2%~10.3%、2.9%~10.8%。方法检出限为4.0μg/kg,定量限为12.0μg/kg,符合农药多残留检测要求。该方法操作简便快速,适用范围广,净化效果较好,可用于菊花中25种有机氯农药多残留量检测。
A gas chromatographic method for determination of 25organochlorine pesticides in Flos Chrysanthemiwas established.Ultrasonic extraction was processed for the sample by using acetone/ petroleum ether(1∶1)as the extract solvent.Then the extracts were cleaned up by sulphuric acid and separated by HP-5and DB1701dual capillary column and detected by GC-ECD.Results show that the recoveries were 69.9%-113.9%,69.4%-100.3%,70.1%-103.1%,and the relative standard deviation were 2.3%-11.9%,3.2%-10.3%,2.9%-10.8%.The limit of detection(LOD)of the method was 4.0 μg/kg,and the limit of quantity(LOQ)was 12.0μg/kg.The method has advantages of simple operation,fast and wide applicability and can be used in determination of organochlorine pesticide residues in Flos Chrysanthemi.