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UM Dissertations & Theses Collection (澳門大學電子學位論文庫)

Title

Chromatographic analysis of active components in Semen Ziziphi Spinosae

English Abstract

The seeds of Semen Ziziphi Spinosae (Suanzaoren) were used as a sedative medicine in China. It has the central depressant action. Generally, sapinosides and flavonoids were considered as major active components in Suanzaoren. However, some studies suggested that Suanzaoren oil was also favorable for its sedative and hypnotic effects. T(CMST(CAT(Cl) Up to date, most studies of active components in Suanzaoren focused on saponins. Jujuboside A and B have already been used as markers for quality control of Suanzaoren materials based on Chinese Phamacopoeia (2005). However, few quantitative and qualitative analyses of flavonoids, one kind of active component in Suanzaoren, were performed. In addition, fatty oil (~32%) is one of major components in Suanzaoren, and the relative contents of fatty acids in the oil were usually analyzed as methyl esters by GC-MS after saponification and methylation. In our studies, an HPLC-ELSD method was developed for the simultaneous determination of two major kinds active components, saponins and fatty acids, in Suanzaoren. It is a novel, rapid and simple method for quantification, especially for the analysis of fatty acids. The thesis consists of 6 Chapter. Chapter 1 was a brief review on active components in Suanzaoren. This part introduced the developments of chemical components, pharmacological activities and quality control methods of sapinosides, flavonoids, fatty oil, respectively. Chapter 2 was the isolation and identification of flavonoids from Suanzaoren. Chapter 3 was GC-MS analysis of the fatty acids in Suanzaoren, which was a conventional method for fatty acids analysis. Although the results obtained were acceptable, the process of derivatization before GC-MS analysis was often undesirable and sensitive to reaction conditions. To simplify the analysis method, an HPLC-ELSD method for simultaneous determination of two major kinds of active components named saponins and fatty acids in Suanzaoren was developed. And the details were described in Chapter 4. Furthermore, Chapter 5 was the qualitative analysis of three major kinds of active components in Suanzaoren by using LC-MS, which simultaneously detected all the major active components in Suanzaoren. Finally, Chapter 6 was the comparison and evaluation of GC-MS and HPLC-ELSD methods for fatty acids assay. The results showed that HPLC-ELSD was a simpler method, where methylation was not necessary. In sum, the chromatographic analysis of active compounds in Semen Ziziphi Spinosae by GC-MS, HPLC-ELSD and LC-MS had been studied. The résults showed that HPLC-ELSD was a simple method for analysis of components such as saponins and fatty acids in Suanzaoren. Anyway, the studies mentioned above will be helpful' to the quality control of Suanzaoren. Key words: Semen Ziziphi Spinosae(Suanzaoren), GC-MS, HPLC-ELSD, LC-MS, chromatographic analysis, quality control

Chinese Abstract

中药酸枣仁 (Semen Ziiphi Spinosae) 具有中枢抑制作用,多被用作镇静催眠药。通常认为酸枣仁的主要活性成分是其中的皂苷和黄酮类组分。但有研究豆 示:酸枣仁油对于其镇静催眠的作用也有一定的贡献。酸枣仁皂苷 A 和酸枣仁皂苷 B,作为酸枣仁当中的有效成分,己被 2005版《中国药典》用作酸枣仁药材的质量控制指标。通过对文献的查阅和综述发现,酸枣仁活性成分的研究多集中于其中的皂苷类成分。而作为酸枣仁另一活性成分的黄酮类成分的研究却非常有限,对于酸枣仁中含量高达 32%的脂肪油分析,也 仅是甲酯化后应用 GC-MS 测定其相对含量。 基于上述原因,我们建立了一种 HPLC-ELSD 方法,可同时分析酸枣仁当中的皂苷和脂肪酸这两类主要的活性成分。此方法快速、简便,特别适用于分析脂肪酸。论文共分为 6章。第一章是有关酸枣仁中活性成分的文献综述,将分别介绍皂苷、黄酮和脂肪油这三大类成分的化学组成、药理活性及质量控制方法。第二章则是分离及鉴定黄酮苷类物质,这是为了后续的研究做准备。GCMS 是脂肪酸的常规分析方法,第三章中,我们首先进行了酸枣仁中脂肪酸的 GC-MS 分析。虽然最终得到的结果尚可以接受,但是柱前的衍生化步 骤繁杂,影响因素多。 为此,我们试图改进方法以避免衍生化的步骤,鉴于 ELSD 对无紫外吸收物质的检测优势,建立了一种同时测定酸枣仁当中的皂苷和脂肪酸这两类主要成分的 HPLC-ELSD 方法,具体的内容见第四章。第五章是运用 IC-MS 定性分析酸枣仁中三类主要活性成分,实现了同时监测酸枣仁中的全部主要活性成分。第六章 是对于脂肪酸的 GC-MS 和HPLC-ELSD 分析的比较研究,结果提示:HPIC-ELSD 是一分析脂肪酸类成分的简便方法。总而言之,我们基于对酸枣仁中主要活性成分的色谱研究结果将有助于酸枣 仁的质量控制。 关键词:Semen Ziziphi Spinosae (酸枣仁),GC-MS,HPLC-ELSD, LC-MS,质量控制,色谱分析

Issue date

2005.

Author

Zhao, Jie

Faculty
Institute of Chinese Medical Sciences
Degree

M.Sc.

Subject

Materia medica -- China -- Analysis

Chromatographic analysis

Supervisor

李紹平

王一濤

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Location
1/F Zone C
Library URL
991008380199706306