摘要
目的:建立中药材中19种有机氯农药残留的毛细管气相色谱分析方法。方法:样品用醋酸乙酯超声提取并经串联Carbon-GCB-Florisil固相萃取柱净化,以不分流进样方式,用DB-35弹性石英毛细管柱,程序升温(柱初始80℃,40℃.min-1升至200℃,5℃.min-1升至300℃,保持2 min),进样口温度300℃,并用电子捕获检测器进行检测,检测器温度300℃,外标法计算含量。结果:方法的平均回收率为80.06%～124.0%,RSD 3.5%～10.7%。所测定的苦参、延胡索、菊花、钩藤、郁金5种中药材均含有不同程度的农药残留。结论:该方法快速、简便、准确,适用于中药中有机氯类农药残留的检测。
Objective： To develop a capillary gas chromatographic method for detection and determination of 19 organochlorine pesticide residues in Chinese herbal medicines. Method： Sample was extracted with ethyl acetate using an ultrasonic bath, and cleaned up with solid phase extraction cartridges, Carbon-GCB-Florisil in series. Analysis was carried out on a fused silica capillary column （ DB-35, 0.53 mm x 30 m, 0.25 ixm film）. The temperature program was as follows： initial temperature at 80 ~C , the 40 ~C ＂min-I to 200 ~C , then 5 ~C ＂min-1 to 300 ~C , and kept for 2 min. The injection port temperature was set at 300 ~（2. The injection mode was splitless. The temperature of electron capture detector was set at 300 ~C. The content was calculated with external standard method. Result： The average recoveries of 19 organochlorine pesticides were from 80.06% to 124.0% , and RSD values were from 3.5% to 10.7%. The content of the organochlorine pesticides in five Chinese herbal medicines, Uncariae Ramulus Cununcis, Chrysanthemi Flos, Sophorae Flaveseentis Radix, Corydalis Rhizoma and Curcumae Radix, was determined. Conclusion： The method was simple, fast, accurate, and can be used for detection and determination of organochlorine pesticide residues in Chinese herbal medicines.
出处
《中国实验方剂学杂志》
CAS
北大核心
2013年第4期96-99,共4页
Chinese Journal of Experimental Traditional Medical Formulae
基金
重大新药创制项目(2009ZX09301-005
2009ZX09308-003)
中药质量控制技术国家工程实验室资助课题(2009ZX09308-003)
中国中医科学院自主课题(Z02063)
关键词
中药材
有机氯农药
毛细管气相色谱法
电子捕获检测器
capture detectorChinese herbal medicines
organochlorine pesticide
capillary gas chromatography
electron
