超声提取气相色谱法测定保健品中.docVIP

超声提取-气相色谱法测定保健药品中15种有机氯农药残留量( 张勇1，刘玉波1，2，陈丽丽1，夏品华1,李存雄1＊，张明时1，2＊ (1 贵州师范大学贵州省山地环境信息系统和生态环境保护重点实验室，贵州 贵阳 550001 2 贵州莱德色谱技术开发有限公司，贵州 贵阳 550001) 摘 要：建立了保健药品中15种有机氯农药残留量的测定方法。样品经丙酮、二氯甲烷、石油醚超声提取，提取液过弗洛里硅藻土层析柱净化，采用电子捕获检测器测定15种有机氯农药残留量。15种农药的检出限为0.091～0.621ng·Kg-1，此方法3个水平的加样回收率为80.5～117.4%之间；相对标准偏差为1.2～12.4%之间。本方法重复性好、操作简单，可作为保健药品中有机氯农药残留量的检测方法。 关键词：超声提取；气相色谱；保健药品；有机氯 中图分类号： 文献标识码： 文章编号：Determination of 15 Organochlorine Pesticide Residues in Health Care Medicines by UE/GC ZHANG Yong1, LIU Yu-bo1,2, CHEN Li-li1, XIA Pin-hua1, LI Cun-xiong1* , ZHANG Ming-shi1,2* (1 Key Laboratory for Information System of Mountainous Area and Protection of Ecological Environment of Guizhou Province，Guizhou Normal University, Guiyang 550001,China; 2 Guizhou Ryder Chromatography Technology Development Co., Ltd., Guiyang 550001, China) Abstract: Objective To establish a method of detecting 15 organochlorine pesticide residues in health care medicines, α-BHC, PCBN, γ-BHC, heptachlor, aldrin, β-BHC, δ-BHC, heptachlor epoxide, PP’-DDE, dieldrin, endrin, OP’-DDT, PP’-DDD and PP’-DDT were discussed. Methods Samples were successively extracted by acetone, dichloromethane and petroleum ether, purified by Florisil column and detected by GC-ECD. Results The detection limits of 15 organochlorine pesticide residues were 0.091~0.621 ng·Kg-1, the recovery in three different levels were 80.5~117.4% and relative standards were 1.2～12.4%. Conclusions The method is simple and accurate with a good reproducibility , so it is suitable for the determination of organochlorine pesticide residues in health care medicines. Key words: ultrasonic extraction (UE); gas chromatography (GC); health care medicines; organochlorine pesticide residues 随着社会的发展，人们生活水平的不断提高，市场上的保健药品也越来越多，保健药品其功能强大正逐渐进入人们的家庭。有机氯农药在我国虽然已经停止生产和使用，但由于其半衰期较长，因而在食品、土壤和中草药中的检出率仍然非常高[1-3]。保健药品中大多含有中草药成分，其卫生质量是否合格显得尤为重要，只有掌握保健品中有机氯农药残留的状况，才能对市场上保健药品的质量和安全进行监督和评价。我国还没有规定专门针对保健药品中有机氯农药残留的国标方法，关于中成药和中药材中有机氯农药残留的测定较多[45]，而关于保健药品中15种有机氯农药