Abstract The shelf life of medicine means that the duration could ensure its quality under special storage conditions, which is an important parameter for the safety and efficacy of the medicine. However, there is no shelf life for Chinese crude drug until now. Therefore, the quality control is a big problem. This thesis based on the study of Danggui (Angelica sinensis), a commonly used Chinese medicine, to explore the essentiality and feasibility of establishing the shelf life for Chinese crude drug. There are three chapters in this thesis. The research background of this study was introduced in Chapter 1, which included the current status of Chinese crude drug's hoarding and the empirical methods of stability. Chapter 2 developed a rapid, accurate with high repeatability HPLC method for simultaneous determination of ferulic acid, coniferyl ferulate, E/Z-ligustilide and E/Z-butylidenephthalide in Angelica sinensis. Sample preparation including ultrasonication, superctitical fluid extraction (SFE), hydro distillation (HD), accelerated solvent extraction (ASE) and decoction were also optimized. Chapter 3 explored the shelf life based on the content variation of coniferyl ferulate and Z-ligustilide in Angelica sinensis using the classic homeothermia method. The validity of the predict value was evaluated by mimic practical storage. The results show that the homeothermia method is a potential approach for predicting the shelf life of Chinese medicines. In a word, the shelf life of Angelica sinensis has been investigated, and its significance for ensuring the safety and efficacy of Chinese crude drug was also been discussed. Simultaneous determination of six components in Danggui by HPLC-DAD were developed, which is helpful to control the quality of Angelica sinensis. Five extraction methods including HD, PSE, SFE, ultrasonication and decoction had their characteristics for extraction of chemical components in Danggui. Key words: Chinese crude drug, shelf life, classic homeothermia method, Angelica sinensis, coniferyl ferulate, ligustilide

摘要 药品的有效期是指药品在一定的贮存条件下,能够保证质量的期限,它是保证 药品安全有效的重要参数。但目前还没有针对中药材保质期的标准,因而中药材 管理无据可依,质量参差不齐,也使得现有中药成方制剂的有效期制定科学依据 不足,严重影响中药的临床疗效,是阻碍中药走向国际化的瓶颈。 本研究针对中药材保质期问题,以常用中药材当归为例,基于其主要化学成 分的含量变化,应用经典恒温法对当归药材保质期进行预测,以探讨建立中药材 保质期的必要性和可行性。 全文共分为三章。第一章介绍了本课题的研究背景,从中药材的贮藏现状分 析了对中药材建立保质期的必要性,同时,综述了稳定性实验方法的研究进展。 第二章建立了当归主要化学成分的HPLC 分析方法,并优化比较了不同提取方 法的影响,为当归药材保质期考察做准备。具体包括:对当归药材化学成分和药 理作用进行了简要的综述,确定分析检测的六个指标性成分:阿魏酸、阿魏酸松 柏酯、E/Z-藁本内酯和E/Z-3-丁烯基苯酞;建立了同时测定当归中这六种有效成分 含量的高效液相色谱法,结果表明该方法准确简便,具有良好的重复性和稳定性; 优化了超声提取法、超临界流体萃取法(SFE)、加压溶剂提取法(ASE)、水蒸气蒸 馏法和传统煎煮法对当归药材中主要化学成分的提取,并比较了五种方法提取的 特点。 第三章是本文的重点内容,考察了当归药材中六种有效成分的稳定性,选择 以阿魏酸松柏酯和Z-藁本内酯为指标,应用经典恒温法对当归药材保质期进行了 预测,并对预测结果进行了实验验证,结果基本一致。在此基础上,对中药材建立 保质期存在的问题进行了较系统的讨论,提出了可行的研究方案。 总之,本文针对提出的建立中药材保质期的构想,以常用中药材当归为例进行 了初步研究,为中药材建立保质期提供了有益的参考;建立了同时测定当归药材 中六个主要有效成分含量的HPLC方法,有利于提高当归药材的质量控制水平; 研究还发现,不同提取方法得到的当归提取物成分明显不同,为进一步研究提供 了线索。 关键词:中药材,保质期,经典恒温法,当归,阿魏酸松柏酯,藁本内酯