气相色谱-质谱法测定太子参药材中有机氯类农药残留  

GC-MS method for the determination of residues of organochlorine pesticides in Radix Pseudostellariae

作　　者：徐晓琴[1] 李庆玲[2] 韩超[1] 黎先春[2] 王小如[1,3] 

机构地区：[1]厦门大学化学化工学院 [2]国家海洋局第一海洋研究所 [3]国家海洋局第一海洋研究所青岛现代分析技术及中药标准化重点实验室,青岛266061

出　　处：《药物分析杂志》2007年第9期1348-1351,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：国家科技部攻关计划项目(No.2003BA759C)

摘　　要：目的:研究太子参药材中15种有机氯类农药:六六六(包括α-,β-,γ-,δ-BHC)、滴滴涕(包括 p,p′-DDE,p,p′-DDD,p,p′-DDT,o,p′-DDT)、五氯硝基苯、七氯、艾氏剂、硫丹、狄氏剂、异狄氏剂、甲氧氯的毛细管气相色谱-质谱(GC-MS)测定方法。方法:太子参样品经正己烷-丙酮(8:2)振荡提取、Florisil 硅土色谱柱净化处理,用 HP-5MS 弹性石英毛细管柱(30 m×0.25 mm×0.25 μm)经程序升温(初温50℃,以30℃·min^(-1)升至200℃并保持3 min,以30℃·min^(-1)升至230℃并保持3 min,以20℃·min^(-1)升至250℃并保持3 min)技术分离,并用质谱检测器检测。确认含有该种农残的条件:1.可疑色谱峰的定量离子和参比离子提取质量色谱图的保留时间都和标准品一致;2.定量离子和参比离子响应强度的比值和标准品相比相对标准偏差在±15%以内。结果:15种有机氯农药获得了良好的分离,线性关系良好,相关系数为0.9807～0.9963;柃出限为2.0～36 ng·g^(-1);平均加样回收率为70.7%～124%,RSD 为0.9%～11%。所测样品中含有痕量的农药残留。结论:本法简便、准确,净化效果好,可用于太子参药材中15种有机氯农药残留量的检测。Objective：To develop an GC -MS method for the determination of residues of 15 organochlorine pesticides （OCPs） [ including alpha, beta, gamma, and delta isomers of benzenehexachloride （ BHC ）, pentachloronitrobenzene （ PC NB ）, heptachlor, Aldrin, endosulfan, p, p＇ - DDE, Dieldrin, Endrin, p, p＇ - DDD, o, p＇ - DDT,p, p＇ - DDT and methoxychlor] in Radix Pseudostellariae （Taizishen in China）, a famous medicinal herb in China. Methods： Raw plant samples were extracted with mixed solvents of hexane and acetone, and then cleaned up by a column packed with Florisil. The capillary column used was HP -5 MS （30 m × 0.25 mm × 0.25 μm）. The chromatographic conditions were as follows： initial temperature 50 ℃ ,30 ℃ · min^-1 to 200 ℃ （hold 3 min）,30 ℃ · min^-1 to 230 ℃ （ hold 3 min）, 20 ℃ · min ^- 1 to 250 ℃ （ hold 3 min）. Pesticides in samples are identified when the following criteria are met：the chromatographic peaks of both ions for the unknown and the standard sample must coincide at the same retention time and the ratio between the two selected ions must be the same with a tolerance of ± 15 %. The pesticide residues were determined based on internal standard method. Results：The method showed good linearity with correlation coefficients ranging from 0. 9807 to 0. 9963. The detection limits for OCPs range from 2.0 -36 ng · g^-1. The average recoveries were 70.7% - 124% with corresponding RSD of 0.9% - 11%. The resuits show that some samples contain OCPs, but the concentration levels are below the regulatory limits of China National Standards. Conclusion：The method is easy to operation, and with good precision and reproducibility.

关 键 词：太子参 有机氯类农药 气相色谱 质谱 

分 类 号：R917[医药卫生—药物分析学]