Application of Chromatographic Method in Quality Control of Traditional Chinese Medicine

摘要中药是一个非常复杂的体系，如何全面有效的对中药质量进行控制是中药现代化的一个重要方面，也是中药规范化、走向世界的关键技术之一。目前，中药质量控制中存在的最大问题是中药的多指标控制水平低、质与量相关性差，因此，在了解和掌握各种现代化学分离分析方法的基础上，针对性地创建新方法，确定并分离提取中药有效成分，并获取其定性定量信息，是现阶段中药质量控制研究的核心。基于此，本论文工作以甘草、丹参、泽泻三味中药材为研究对象，探索了中药有效成分群的分离提取和色谱分离分析方法，发展了薄层色谱多次展开新方法，结合指纹图谱技术和化学计量学方法对药材质量进行了评价。其意义在于为建立此三味中药之研究开发及生产的标准...Abstract Traditional Chinese medicine (TCM) is a very complex system, a comprehensive and effective analytical technology for the quality control of TCM is an important area of research in the modernization of TCM. In this thesis, the extraction of active components in TCM and the chromatographic separation of the active components group have been explored. A novel TLC multiple development...学位：理学硕士院系专业：化学化工学院化学系_分析化学学号：20022501

The Application in GAP Production and Quality Control of glycyrrhiza uralensis Fisch.by TLC Fingerprint Spectrum

目的　研究甘草药材的薄层色谱指纹图谱 ,为科学评价及有效控制其质量提供可靠方法。方法　样品经预处理后点于硅胶 GF2 54预制板上 ,以乙酸乙酯 -乙酸 -甲酸 -水 ( 15∶ 1∶ 1∶ 2 )为展开剂 ,于 2 5 4 nm处进行吸收扫描。结果　甘草药材样品得到的薄层色谱指纹图谱有 6个共有峰 ,依此建立的柱状条形码图能快速地对药材品质作出评判。结论　采用 TL C指纹图谱可有效控制 GAP基地甘草的质量。Objective To set up a sensitive and specific TLC method for controlling the quality of glycyrrhiza uralensis Fisch..Method The sample solution was applied to the commercial pre-coated 20×10 cm silica gel F 254 plate (Merck) modified by 1% sodium hydroxide, ethyl acetate-formic acid-ethanoic acid-water(15∶1∶1∶2) as the solvent system, and quantitative analysis was carried out using UV absorptive scanning at 254nm. Result The TLC-FP of glycyrrhiza uralensis Fisch.showed 6 characteristic common peaks. The pole graph based on the height of common peaks can be conveniently used to evaluate the quality of different samples. Conclusion Quality of GAP glycyrrhiza uralensis Fisch. can be controlled effectively by TLC fingerprint.国家自然科学基金 2 0 0 3重点项目 ( 2 0 2 3 5 0 2 0

Study on the TLCS fingerprint of Glycyrrhiza uralensis Fisch.

目的研究甘草药材的薄层扫描指纹图谱 (TLCS FP) ,为科学评价及有效控制其质量提供可靠方法。方法采用 1% (w)氢氧化钠浸渍硅胶GF2 5 4预制板 (Merck) ,醋酸乙酯 甲酸 冰醋酸 水(V∶V∶V∶V =15∶1∶1∶2 )为展开剂 ,2 5 4nm紫外吸收扫描。结果 14批甘草药材样品得到的TLCS指纹图谱有 6个共有峰 ,聚类分析结果正品甘草药材有较好的相似度 ;三维图谱可对不同产地的甘草药材质量进行直观比较。结论该TLCS FP可用于甘草的真伪鉴别和质量评价Objective To establish a sensitive and specific TLCS method for controlling the quality of Glycyrrhiza uralensis Fisch..Method The characteristic TLCS chromatogram was obtained by using pre-coated 20 cm×10 cm silica gel 60F254 plate (Merck) modified by 1% sodium hydroxide,ethyl acetate-formic acid-acetic acid-water(15∶1∶1∶2) as the solvent system,and quantitative analysis was carried out using UV absorptive scanning at 254 nm.Result The TLCS-FP of Glycyrrhiza uralensis Fisch.,showing 6 characteristic peaks,was established by 14 lots of Glycyrrhiza uralensis Fisch..By cluster analysis and similarity calculation,the similarity of the positive samples was very high.3D graph was selected to compare the results.Conclusion This method can be used to identify and evaluate the quality of Glycyrrhiza uralensis Fisch..国家自然科学基金 2 0 0 3重点项目 (2 0 2 35 0 2 0

Dynamic study of zexie by HPLC fingerprinting technique

应用指纹图谱技术,结合指标成分测定,采用高效液相色谱法,乙腈-水梯度洗脱,流速1.0 mL/min,柱温20℃,色谱图光谱采集范围200~800 nm,探讨了泽泻动态积累的规律。以泽泻标准对照药材为参照,用指标成分24-乙酰泽泻醇A和23-乙酰泽泻醇B进行了定位和测定,找出了21个共有峰,其中12号和20号峰分别为24-乙酰泽泻醇A和23-乙酰泽泻醇B。结果表明:泽泻样品指纹图谱及指标成分测定可为泽泻的最佳采收期提供科学依据。Fingerprints of 10 samples of zexie collected at different harvest times were studied by high-performance liquid chromatography with acetonitrile-water gradient elution,flow-rate of 1.0 mL/min,column temperature of 20 ℃,acquisition wavelength of 200～800 nm,authorized control samples as reference,fingerprints were positioned with 24-acetyl-alisol A and 23-acetyl-alisol B as the index components.21 common peaks were analyzed,the 12~(th) and 20~(th) peaks were 24-acetyl-alisol A and 23-acetyl-alisol B respectively.The result showed that combined with content determination,the HPLC fingerprint of dynamic samples of zexie can be used to determine the optimal harvest time for zexie GAP bases.2001年度福建省重大科技项目-福建省地道中药材GAP研究及其标准化生产示范基地建设项

Quality Assessment of Radix Salvia Miltiorrhiza (Danshen) by TLC Fingerprinting Technique

利用薄层色谱(TLC)技术对中药材丹参的有效成分进行了指纹图谱分析.以不同等级的中江丹参和不同采收期的丹参、南丹参为分析对象,采用适宜的水溶性及脂溶性成分提取方法和TLC分析条件,可获得其相应的TLC图像及色谱图.通过对不同丹参药材的色谱图像的分析,结合化学计量学方法对其各主要指标成分的信息进行提取,初步构建了丹参的TLC指纹图谱.结果表明,在254 nm波长下获取脂溶性和水溶性成分共7个共有指纹峰,各峰相对比移值(Rf)和峰面积的相对标准偏差分别小于1.7%和4.0%.通过对薄层色谱斑点的Rf值、斑点颜色和大小的比较,并进行主成分分析和聚类分析,实现了对不同等级的丹参进行归属,并确立了最佳采收期.本实验建立的薄层色谱指纹图谱方法具有较高的稳定性、良好的精密度和重现性,可用于丹参药材的质量评价和控制.The purpose of this study is to develop and apply the thin layer chromatography(TLC) technique to the fingerprinting studies of Danshen(Radix Salvia Miltiorrhiza) drugs.A range of Danshen samples with different commercial grades or harvested after different growing time was analyzed for quality assessment and regulatory purposes.And the compositional variations of these authentic Danshen drugs were investigated using an analytical protocol involving water or organic solvent extractions,followed by TLC assay of the extracts,and subsequent TLC fingerprinting analysis by image comparison combined with chemometrics methods.The analytical performances of the method were evaluated by examining the stability,precision and reproducibility,respectively.Excellent results were observed and the RSDs of relative R_f values and peak areas were respectively less than 1.7% and 4.0%.The analysis results obtained suggested that a total of seven common peaks were identified in the TLC chromatograms under the 254 nm detection wavelength.Based on the comparison of the R_f values of the common peaks,the depth and size of the TLC spots and in combination with cluster analysis and principal component analysis(PCA),the attribute of quality grading and optimal harvest time of the Danshen material were identified.Thus,the developed TLC chromatographic fingerprinting method is considered as an useful and effective tool for the quality control of the Danshen drug material.科技部"九五"攻关计划中药现代化重中之重项目:中药现代化生产中重金属测定的标准化及质量控制(99-929-02-13);; 香港创新科技署与香港新世界生物科技有限公司联合资助项