【作者】 辛龙涛；

【导师】 夏之宁；

【作者基本信息】 重庆大学 ， 药物化学， 2005， 硕士

【摘要】 中药经过长期的临床实践证实,具有确切的疗效,合理运用可减少或避免毒副作用。但由于缺乏客观、严格的质量控制、检验标准和可靠、系统的科学实验证实其有效性和安全性,中药至今未能进入国际医药主流市场。将现代化的科学分析技术用于传统中药的现代化研究,具有重要的实际意义。毛细管电泳技术是近年发展起来的一种新的分析手段,具有高效、快速、样品用量少等优点。非水毛细管电泳由于使用了有机溶剂作为分离介质,具有一些常规毛细管电泳所不具备的优势,拓宽了毛细管电泳的应用范围,在分析水不溶性物质方面具有独到的优势。本文首先综述了近年来毛细管电泳在中药领域的研究现状以及非水毛细管电泳用于中药分析的现状。然后将毛细管电泳技术用于中药厚朴和吴茱萸的成分分析中,建立了两种不同的毛细管电泳方法。研究的主要内容及结果如下: 1. 以缓冲液加入β-CD 为添加剂的毛细管区带电泳方法,用于厚朴药材及其制剂的分析。优化了厚朴提取物的分离条件,考察了缓冲溶液浓度、pH 值、β-CD的添加浓度对分离的影响,确定了最佳的分离缓冲溶液组成为30 mmol/L 硼砂和2.4 mmol/L β-CD,pH 值为9.48;推测出和厚朴酚的二级离解常数pKa2 的范围为9.94-10.83;在优化的分离条件下,测定了厚朴药材和藿香正气口服液中和厚朴酚的含量分别为3.42-5.98 mg/g、0.021 mg/mL,和厚朴酚的线性范围是0.020-0.405 mg/mL,其线性相关系数R=0.998(n=5),加样回收率为98.4-103.5%,RSD 为3.2-5.7%(n=3)。2. 建立了非水毛细管电泳用于吴茱萸中吴茱萸次碱的分离测定的方法。考察了影响电泳分离的各因素如缓冲溶液的浓度、用于调节酸碱度的乙酸的添加比例及用于调节电渗流的乙腈的添加比例,最后优化的分离缓冲溶液的组成是40 mmol/L NH4Ac 的甲醇溶液,其中含有30%的乙腈和10%的乙酸。在优化的分离条件下,对吴茱萸药材中的吴茱萸次碱含量进行了测定,吴茱萸次碱的线性范围是0.0230～0.460 mg/mL,其线性相关系数R=0.9973(n=7),加样回收率为106.3%(n=3)。更多还原

【Abstract】 Traditional Chinese Medicine (TCM) has been proved to have definite therapeutic effects through clinical application for a long time, and most TCM have slightly or no side effect if administered reasonably. Because of deficiency in objective and strict quality controlling-testing criterion, reliable and systematic scientific experiments to verify its validity and security, TCM is still kept out of the prevailing international medicine market. It is of practical significance to apply this scientific method to modern researches of TCM. As a new advanced method of separation and analysis, Capillary electrophoresis (CE) has been used in the field of analytical chemistry, with such merits as high efficiency, speediness and low cost. By use of organic solvents as separation media, nonaqueous capillary electrophoresis (NACE), which expands the application of CE, has some merits that can’t be found in conventional CE. It is provided with original advantages in analyzing materials with poor aqueous solubility. There are mainly two parts in this thesis. In the first part, the development of researches in TCM with CE and NACE was reviewed. In the second part, the content of two kinds of TCM was analyzed by CE and NACE, respectively. The main research contents and conclusions are mentioned as below: 1. A capillary zone electrophoresis method modified with β-cyclodextrin (β-CD) was developed for the purpose of determining the content of honokiol in Cortex Magnoliae Officinalis and Cortex Magnoliae Officinalis-containing preparation. The factors relevant to the running buffer and their effects on separation were investigated. The buffer solution composed of 30 mmol/L sodium borate and 2.4 mmol/L β-CD was found to be the most suitable electrolyte for separation. The second order dissociation constant range of honokiol was estimated. The content range of honokiol in Cortex Magnoliae Officinalis and was 3.42-5.98 mg/g, while the mean content of honokiol in its preparation (Huoxiangzhengqi Oral Liquid) 0.021 mg/mL. A good linear response towards honokiol was found in the range from 0.020 mg/mL to 0.405 mg/mL (R= 0.998, n=5). The recovery ranged between 98.4% and 103.5%. 2. A simple NACE method has been developed for the assay of Rutaecarpine in Evodia rutaecarpa for the first time. Optimum separation of the analytes was obtained using a nonaqueous buffer system with 40 mmol/L ammonium acetate containing 30% acetonitrile and 10% acetate acid. The factors relevant to the running buffer and their effects on separation were discussed. The content of Rutaecarpine in Evodia rutaecarpa was determined. The assay was linear for Rutaecarpine in the concentration range of 0.023-0.46 mg/mL, R=0.9966(n=8). The recovery is 106.3%(n=3).更多还原