固相萃取毛细管气相色谱法测定党参、龙胆中15种有机氯农药的残留量

目的用固相萃取毛细管气相色谱分析方法测定党参、龙胆2种中药材中15种有机氯农药残留量。方法样品以混合溶剂超声提取、Florisil固相萃取小柱净化处理后,采用DB 1701毛细管气相色谱柱分离样品,电子捕获检测器检测,内标法定量。结果15种农药在5~500μg.L-1内具有良好的线性关系,相关系数均大于0.995 0。15种农药3个不同质量浓度的平均回收率为83.1%~110.6%,RSD为3.4%~14.8%。最小检测量为0.08~1.50μg.L-1。被测样品中均含有不同程度的有机氯农药。结论本法可用于中草药党参和龙胆中有机氯类农药的残留量测定。

Determination of organochlorine pesticide residues in Radix Codonopsis, Radix Gentianae by solid-phase extraction and capillary gas chromatography

Objective To use the solid-phase extraction and capillary gas chromatography for the determination of 15 organochlorine pesticide residues(OCPs) in Codonopsis pilosula,Gentiana scabra.Methods Fifteen organochlorine pesticides were extracted from samples with solvents by ultrasonic and clean up by Florisil solid-phase extraction column.Then,the extract was separated by capillary column and detected by electron capture detector.The internal standards were used for quantitative determination.Results Good liner relation was obtained over the range of 5-500 μg·L~(-1).The average recoveries and RSD were in the range of 83.1%-110.6% and 3.4%-14.8% at three organochlorine pesticides levels,respectively.The limits of detection were 0.08-1.5 μg·L~(-1).All the samples showed organochlorine pesticide residues.Conclusions This method has good repeatability and suitable for the analysis of organochlorine pesticide residues in traditional Chinese medicines.