毒性中药天仙子有效成分的液相色谱_质谱法定性定量分析_祁文娟

毒性中药天仙子有效成分的液相色谱－质谱法定性定量分析

祁文娟1，王兆基2，吴志成2，刘秋铭2，粟晓黎1，林瑞超1*，郑秀云3，冯国培3（1．中国食品药品检定研究院，北京100050；2．香港特别行政区政府化验所；3．香港中文大学）

摘要目的：总结中药天仙子毒性毒理，针对现有质量标准检定方法建立一个专属性较强的毒性药效成分定性与定量分析方法。方法：采用Restek Allure PFP Propyl（2.1mmˑ100mm，5μm）色谱柱，流动相为乙腈－醋酸铵缓冲液（20ʒ80），流速200μL·min－1，分流比率9ʒ1，进样量10μL；正离子多反应监测模式监测，扫描范围为m/z200 350的高效液相色谱－质谱联用方法，对天仙子中毒性药效成分进行定性鉴别和含量测定。结果：利用东莨菪碱及阿托品的液相色谱分离及其特征质谱－质谱图，对3批不同产地药材进行定性定量分析，总莨菪碱（以阿托品计）含量范围为0.02% 0.05%之内。结论：本文建立的液相色谱－质谱联用技术具有专属性强等优点，可为质量标准修订提供参考。

关键词：中药材；莨菪；天仙子（莨菪子）；东莨菪碱；阿托品；高效液相色谱－质谱联用；毒性药效成分；定性鉴别；含量测定；标准修订

中图分类号：R917文献标识码：A文章编号：0254－1793（2012）04－0599－04

HPLC－MS qualitative and quantitative analysis for poisonous

traditional Chinese medicine Hyoscyami Semen

QI Wen－juan1，WONG Siu－kay2，NG Chi－shing2，LAU Chau－ming2，

SU Xiao－li1，LIN Rui－chao1*，CHENG Sau－wan3，FUNG Kwok－pui3

（1．National Institutes for Food and Drug Control，Beijing100050，China；

2．Government Laboratory，HKSAR，China；3．The Chinese University of Hong Kong，China）

Abstract Objective：To review the toxicity and pharmacology actions of a commonly used potent Chinese medici-nal material，Hyoscyami Semen．To establish a highly selective analytical method for the qualitative and quantitative analysis of the toxic and active compounds of Hyoscyami Semen with reference to existing quality control methods．Methods：LC－MS/MS technique which was performed on Restek Allure PFP Propyl（2.1mmˑ100mm，5μm）column with acetonitrile－ammonium acetate buffer solution（20ʒ80）as the mobile phase at flow rate of200μL·min－1with split ratio9ʒ1，and positive ion multiple reaction monitoring（MRM）mode，scanning the range of m/z 200－350was employed for qualitative identification and quantitative determination of the toxic and active com-pounds for Hyoscyami Semen．Results：With the use of liquid chromatography separation and MS/MS spectrum characteristics，scopolamine，atropine and other related alkaloids present in Hyoscyami Semen could be identified and quantified，respectively．The method was applied to the analysis of3batches of herbs collected from different sources and the total scopolamine and atropine content was found in the range of0.02%－0.05%（calculated as at atropine）．Conclusion：A highly selective LC－MS/MS method is developed which can serve as a reference method for quality control purposes．

Key words：traditional Chinese medicine；Hyoscyamus niger L．；Hyoscyami Semen；scopolamine（hyoscine）；atro-pine；LC－MS/MS；toxic and active components；identification；assay；standard improvement

天仙子（Hyoscyami Semen）为茄科植物莨菪（Hyoscyamus niger L．）的干燥成熟种子［1］，又名莨菪子，味苦、辛，性温，有大毒。归心、胃、肝经；有解痉镇痛、止咳平喘、安神定惊、收敛固脱的功能；主治

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药物分析杂志Chin J Pharm Anal2012，32（4）*通讯作者Tel：（010）67095307；E－mail：linrch307@sina．com

DOI:10.16155/j.0254-1793.2012.04.013