毛细管气相色谱法测定半夏中20种有机氯农药的残留量  

Determination of Residues of Twenty Kinds of Organochlorime Pesticides in Rhizoma Pinelliae by Capillary Gas Chromatograrhy-Electron Capture Detector

作　　者：隆颖[1] 栗建明[2] 陈浩桉[1] 黄昌杰 谢健鸣[1] 

机构地区：[1]广东省药品检验所,广州510180 [2]广州市药品检验所,广州510160 [3]广州致信药业有限公司,广州511430

出　　处：《中药新药与临床药理》2010年第5期528-530,共3页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：广东省科技计划项目(2007B0314070031);广州市科技局资助项目(2007Z2-E5061)

摘　　要：目的建立半夏中20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FlorisilR固相萃取柱净化,以不分流进样方式,用DB-1701P弹性石英毛细管柱,经柱程序升温(进样口温度:230℃,检测器器温度260℃,柱升温程序初始100℃,8℃/min升至220℃,10℃/min升至250℃,保持12min)技术分离,并用电子捕获检测器进行检测,外标法计算含量。结果方法的平均回收率为84.3%～114.5%,RSD为3.5%～10.7%,所测定样品均含有不同程度的农药残留。结论本方法快速、简便、准确,适用于半夏中有机氯类农药残留的检测。Objective A capilllary gas chromatorgraphic method was developed to determine the residues of 20 kinds of organochlorine pesticides in Rhizoma Pinelliae.Methods The samples were extracted with ethyl acetate by ultrasonography,then were purified by a column packed with Florisil.Non-split stream sampling was carried out on the DB-1701P capillary column（30 m×0.32 mm,0.25 μm）.The column temperature was controlled by computer program：the injector temperature was set at 230 ℃ and the detector temperature at 260 ℃,and the initial column temperature was 100 ℃,with the increase rate of 8 ℃per min to 220 ℃,10 ℃ per min to 250 ℃,holding 12 min.The electron capture detector（ECD）was used.The pesticide residues were calculated by external standard method.Results The average recoveries were in the range of 84.3 %-114.5 % and and RSD was 3.5 %-10.7 %.The organochlorine pesticide residues varied in different samples of Rhizoma Pinelliae.Conclusion The established method is rapid,simple and accurate.It can be used to determine organochlorine pesticide residues in Rhizoma Pinelliae.

关 键 词：有机氯农药 毛细管气相色谱法 半夏 电子捕获检测器法 

分 类 号：R284.1[医药卫生—中药学]