厚朴配方颗粒质量标准及高效液相指纹图谱研究

【作者】 盛燕；

【导师】 夏厚林；

【作者基本信息】 成都中医药大学 ， 药物化学， 2006， 硕士

【摘要】 厚朴配方颗粒为木兰科植物厚朴Magnolia officinalis Rehd．et Wils．的干燥干皮、根皮及枝皮经炮制后制成的配方颗粒，具有燥湿消痰、下气除满之功效，用于湿滞伤中、脘痞吐泻、食积气滞、腹胀便秘、痰饮喘咳。为了控制厚朴配方颗粒的质量，确保临床用药的安全性和有效性，本文对其质量标准、指纹图谱及稳定性进行了研究。 本文系统地研究了厚朴配方颗粒质量控制的各项指标。性状项下，规定本品为棕褐色颗粒，气香，味苦；鉴别项下，分别对厚朴的酚类、生物碱类及挥发油化学成分进行了薄层层析并确定了色谱条件；检查项下，对《中国药典》2005年版一部颗粒剂项下的粒度、水分、溶化性、装量差异、微生物限度及重金属、砷盐、有害元素、农药残留量进行了检查；浸出物项下，对水溶性浸出物、醇溶性浸出物的浸出方法、浸出溶剂进行了研究，并确定它们的含量限度为65％～85％；含量测定项下，采用高效液相色谱法对厚朴酚、和厚朴酚进行了含量测定，进行了供试品溶液制备方法（提取方法、溶剂、时间）的考察，色谱条件（流动相、柱温、检测波长）的考察，系统适应性试验及方法学考察，并确定本品每袋含厚朴以厚朴酚(C₁₈H₁₈O₂)与和厚朴酚(C₁₈J₁₈O₂)的总量计不得少于90.0mg。此外，采用红外光谱法及薄层色谱法对所用辅料——糊精及干姜进行了检查，结果阴性均有一定干扰，故有关辅料检查还有待于进一步研究。 本文参照《中药注射剂指纹图谱研究的技术要求（暂行）》的要求，采用高效液相色谱法对厚朴配方颗粒的指纹图谱进行了研究，包括供试品溶液制备方法（提取方法、溶剂、时间）的考察，色谱条件（色谱柱、流动相、检测波长、柱温、流速）的考察，系统适应性试验、参照物的选择及方法学考察，确定了其指纹图谱共有模式。用“计算机辅助相似性评价系统”对十批中试样品、十二批厚朴药材及十六批姜厚朴药材的指纹图谱分别进行了全谱的相似度评价，结果中试样品指纹图谱相似度系数均大于0.9500，厚朴药材、姜厚朴药材指纹图谱相似度系数均大于0.9000。对厚朴配方颗粒与厚朴、姜厚朴药材之间的相关性进行了评价，结果表明三者之间具有一定的相关性。 本文对三批中试样品进行了6个月的长期留样稳定性试验及加速稳定性试更多还原

【Abstract】 Houpu Dispensing Granule is made from the prepared dried bark of the trunk, root and branch of Magnolia officinalis Rehd. et Wils. It has the effects of eliminating dampness and phlegm, smoothing the flow of qi and removing food stagnation, used for treating retention of dampness in the middle-jiao marked by abdominal distention, nausea, vomiting, stagnation and constipation of indigested food and qi, cough and asthma due to accumulation of phlegm in the lung. In order to control the quality and ensure the security and efficiency clinical use of the Houpu Dispensing Granule, we studied on its quality standard, fingerprints and stability.We studied on the quality control factors systematically. The characters: brown granule, fragrant smelling and bitter tasty. Identification: including the TLC analysis on the Phenols, Alkaloids and Volatile oil and the determination of TLC chromatic parameters . Analysis: all the rules of granule in 《Chinese Pharmacopoeia》 2005ed Vol Ⅰ ,including the granularity, the moisture, the solubility, the content uniformity, the limitation of microorganism, heavy metal, arsenic salt, harmful elements, and pesticide residue; Extractum: including the optimization of the extraction method and the extraction solvent of water-soluble extractives and ethanol-soluble extractives, and finally determined the limitation was 65%-85%.Content Assays: the contents of magnolol and honokiol were assayed by HPLC, the preparation method of the sample （extract method, solvent and time）, the chromatographic parameter（the mobile phase, the temperature, and the test wave-length）,the systematic adaptability test and the methodology were tested, and regulated the content of Houpu , calculated by the magnolol (C₁₈H₁₈O₂) and honokiol (C₁₈H₁₈O₂) ,must not be less than 0.9mg per pouch. Besides, the adjuvant - dextrin and Rhizoma Zingiberis used in processing procedure were identified by IR and TLC, the result demonstrated that even the minus group showed some interference results that more researches were needed on the adjuvant.According to the decree of 《Technical Requirements of Fingerprints of Chinese更多还原