川芎及其制剂的指纹图谱研究

【作者】 生可心；

【导师】 陈发奎；

【作者基本信息】 沈阳药科大学 ， 生药学， 2005， 硕士

【摘要】 本研究以川芎及川芎制剂为研究对象，对其进行了质量评价方法的研究。首先对川芎进行了化学成分研究，共分离得到11个化合物，通过理化性质和光谱数据鉴定其中8个化合物为：阿魏酸(ferulic acid，Ⅰ)，原儿茶酸(protocatechuic acid，Ⅱ)，香草酸(vanillic acid，Ⅲ)，3-正丁基-3-羟基-4，5，6，7-四氢，6，7-二羟基酰内酯(3-n-butyl-3-hydroxy-4,5,6,7-tetrahydro,6,7-dihydro-xyphthalide，Ⅳ)，4-羟基-3-丁基苯肽(4-hydroxy-3-butyl-phthalide，Ⅴ)，Z,Z’-6’,6,7,3’α-二聚藁本内酯(Z,Z’-6’,6,7,3’α-diligustilide，Ⅵ)，胡萝卜苷(daucosterol，Ⅶ)，β-谷甾醇(β-sitosterol，Ⅷ)。其中阿魏酸为川芎制剂的主要活性成分。建立了14个不同来源川芎药材的色谱指纹图谱，用系统聚类分析方法将药材按质量优劣分为两类，其中五批川芎列为推荐品，为川芎制剂中川芎药材产地的选择及合理“勾兑”提供参考。采用HPLC法测定了这14批药材中阿魏酸的含量，结果阿魏酸在20～10μg／ml范围内呈线性关系(r=0.9999)，平均回收率为98.5％(RSD=1.19％)。所建立的测定方法简便、重复性好，为评价川芎质量提供了定量依据。以阿魏酸、天麻苷、天麻苷元为指标成分，建立了鉴别川芎制剂中川芎和天麻药材的TLC鉴别方法。采用同药材相同方法对川芎制剂中阿魏酸的含量进行了测定，为评价该制剂质量提供了定量依据。根据川芎制剂的制备工艺，本品除含有阿魏酸、天麻苷、天麻苷元外，还含有多种酚酸类、苯肽类成分，为全面控制其质量，本文根据《中药注射剂指纹图谱研究的技术要求》，建立了川芎制剂及其中间体的HPLC指纹图谱，通过共有模式生成法模拟出对照指纹图谱，分别对其10批样品采用相关系数、夹角余弦和欧氏距离作为测度，进行了相似度计算。结果表明10批样品及中间体的相似度较高。将样品与中间体和药材的指纹图谱进行对照，三者之间的相关性也较好。更多还原

【Abstract】 The article was mainly about the quality assessment of Chuanxiong Preparation and Rhizoma Chuanxiong.To establish the quality control of Chuanxiong Preparation we studied the chemical constituents of Rhizoma Chuanxiong which was the main composition of the prescription. We got 11 compounds, 8 of them were identified as ferulic acid ( I ), protocatechuic acid (II), vanillic acid (III), 3-n-butyl-3-hydroxy-4,5,6,7-tetrahydro, 6,7-dihydroxyphthalide (IV ) , 4-hydroxy-3-butyl-phthalide ( V ) , Z,Z’-6’,6,7,3’a -diligustilide (VI), daucosterol (VII),β-sitosterol (VIII) .The HPLC chromatographic fingerprints of Rhizoma Chuanxiong which were collected from different habitats was established. The Rhizoma Chuanxiong samples were identified with hierarchical clustering analysis and divided into two grades, five of them were recommended. Ferulic acid of 14 Rhizoma Chuanxiong samples was determined by RP-HPLC. The linear range of ferulic acid was 20-100μg/ml (r=0.9999). The average recovery was 98.5% (RSD = 1.19%). Above methods were simple, rapid and with good reproducibility. It provide a quantitative basis for the quality assessment for Rhizoma Chuanxiong.Rhizoma Chuanxiong of Chuanxiong Preparation was identified of ferulic acid and Rhizoma Gastrodiae was identified of gastrodin and p-hydroxylbenzyl alcohol by TLC. Ferulic acid of Chuanxiong Preparation was determined by the same method of Rhozoma Chuanxiong. It provide a quantitative basis for Chuanxiong Preparation.The HPLC chromatographic fingerprints of 10 Chuanxiong Preparation sample and 10 Intermediate sample was established. The similarity analysis method for quality assessment of Chuanxiong Preparation samples was developed. The similarity of them was determined by cosine, correlation and Euclidean and the three different measures were confirmed with each other. The results of analysis were remarkable.更多还原