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不同产地5种中药材安全限量研究——农药残留分析

Study on Safety Limits of Five Chinese Medicinal Materials from Different Producing Areas-Analysis of Pesticide Residues

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【作者】 牛建均刘春艳李开斌谢宇龙立慧姚元贵王亮张丽艳罗君

【Author】 NIU Jianjun;LIU Chunyan;LI Kaibin;XIE Yu;LONG Lihui;YAO Yuangui;WANG Liang;ZHANG Liyan;LUO Jun;Guiyang College of Traditional Chinese Medicine;Anshun Institute for Food and Drug Control;Guizhou Guangjitang Pharmaceutical Company Limited;The First Affiliated Hospital of Guiyang College of Traditional Chinese Medicine;

【通讯作者】 张丽艳;罗君;

【机构】 贵阳中医学院安顺市食品药品检验所贵州广济堂药业有限公司贵阳中医学院第一附属医院

【摘要】 目的:考查不同产地的太子参、野菊花、三七、茯苓、鱼腥草有机氯农药残留情况,了解我国目前中药材农药残留存在的问题,为后续开发利用药材资源提供理论依据和基础。方法:采用气相色谱-电子捕获检测(GC-ECD) Rtx-1701弹性石英毛细管柱(0.25 mm×30 mm×0.25μm),样品经丙酮,二氯甲烷与石油醚混合有机溶剂超声提取,进样口温度230℃,检测器温度300℃;程序升温,初始温度100℃,先以10℃/min升至220℃,再以8℃/min升至250℃保持10 min,外标法计算含量,应用SPSS 22.0软件对数据结果进行统计学分析。结果:9种有机氯的线性关系良好,相关系数均大于0.995;最低检出限为0.00012~0.00057μg/g;检测仪器的精密度良好,RSD均小于5%;检测方法重现性好,RSD均小于8%;回收率范围为94.91~105.09%。5种中药材中均含有滴滴涕,仅有三七中含有五氯硝基苯;参考2015版《中国药典》和《药用植物及制剂外经贸绿色行业标准》(WM-T2-2004)收载的品种项下"农药残留量"部分检查限度,50批中药材检出含有机氯农药残留率占50%,但含量均较低,其中总六六和总滴滴涕超标率分别为10%和6%,50批中药材合格率达84%,整体符合要求。结论:气相色谱检测法简便快捷、分离效果好,能广泛用于中药材有机氯农药残留的检测。

【Abstract】 Objective To investigate the residues of organochlorine pesticides in Radix Pseudostellariae, Wild Ch-rysanthemum, Sanqi, Poria and Houttuynia cordata from different producing areas, to understand the existing pro-blems of pesticide residues in Chinese herbal medicines, and to provide theoretical basis for the subsequent devel-opment and utilization of medicinal materials basis.Methods Gas chromatography-electron capture detection(GC-ECD) Rtx-1701 elastic quartz capillary column(0.25 mm×30 mm×0.25 μm) was used. The sample was ultraso-nically extracted with acetone, dichloromethane and petroleum ether mixed organic solvent to achieve splitless fl-ow. Mode injection, inlet temperature 230 ℃, detector temperature 300 ℃; programmed temperature, initial te-mperature 100 ℃, first 10 ℃/min rose to 220 ℃ then 8 ℃/min rose to 250 ℃ for 10 min, outside the contenttwas calculated by standard method, and the data were statistically analyzed using SPSS 22.0 software.Results The linearrelationship of the nine organochlorines is good, the correlation coefficient is greater than 0.995;the minimum detection limit is 0.00012~0.00057 g/g; the precision of the detection instrument is good,the RSD is less than 5%; the reproducibility of the detection method is good, and the RSD is smaller than 8%; recovery ranged from 94.91 to 105.09%. Drip sputum is contained in all five kinds of Chi-nese medicinal materials, but only hexachloride benzene is contained in Panaxnotoginseng; it is included in the 2015 edition of Chinese Pharmacopoeia and "Green Standards for Foreign Trade of Medicinal Pla-nts and Preparations"(WM-T2-2004). According to the partial inspection limit of "Pesticide Residues" un-der the variety, 50 batches of Chinese herbal medicines detected 50% of organochlorine pesticide residu-es, but the content was low, and the total rate of total sixty-six and total DDT was 10% and 6% res-pectively. The qualified rat of 50 batches of Chinese herbal medicines reached 84%, and the overall re-quirements were met. Conclusion Gas chromatography detection method is simple, rapid, and has good separat-ion effect. It can be widely used in the detection of organochlorine pesticide residues in Chinese herbal medicines.

【基金】 黔科合重大专项([2016]3023号);贵州省国内一流建设学科(中药学)(GNYL[2017]008号);安顺市科技创新平台建设计划项目(安市科平[2017]03);国家中医药管理局中药特色技术传承人才项目(国中医药办人教函[2018]204号);贵州省科技厅贵阳中医学院第一附属医院联合基金项目(黔科合LH字[2015]7801号);贵州省科技支撑计划项目(黔科合支撑[2018]2772)
  • 【文献出处】 中国民族民间医药 ,Chinese Journal of Ethnomedicine and Ethnopharmacy , 编辑部邮箱 ,2019年09期
  • 【分类号】R284.1
  • 【被引频次】6
  • 【下载频次】571
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