Wu Yu-Qiong, Gou Yu-Qiang, Han Jing, Bi Ying-Yan, Feng Shi-Lan, Hu Fang-Di, Wang Chun-Ming
School of Pharmacy, Lanzhou University, Lanzhou 730000, China.
The Second People's Hospital of Gansu Province, Lanzhou 730000, China.
J Pharm Anal. 2011 May;1(2):119-124. doi: 10.1016/S2095-1779(11)70021-1. Epub 2012 Jan 30.
An approach was proposed to evaluate preparation technology by means of fingerprint-peak matching technology of high Performance liquid chromatography with diode array detector (HPLC-DAD). Similarity and hierarchical clustering analysis (HCA) were applied to identify the 15 batches of Xiaochaihu granules from different manufacturers and our laboratory, and peak pattern matching between the composite formulae and Chinensis, which was one of the main ingredients of Xiaochaihu granules, was utilized to evaluate the preparation technology of Xiaochaihu granules via the indexes of the relative deviation of retention time (RT) and UV spectrum feature similarity of their corresponding peaks. Eleven matching peaks were found between Xiaochaihu granules and Chinensis. However, the saikosaponin A and saikosaponin D, which are the important active components in Chinensis, were not found in Xiaochaihu granules from any manufacturers. The peak areas of 11 characteristic peaks of Xiaochaihu granules samples formed a matrix of 11 × 15. The result of HCA showed that Xiaochaihu granules samples were divided into four kinds of category. Xiaochaihu granules samples from the same manufacturer were basically clustered of the same category. The results suggested that the saikosaponin A and saikosaponin D are prone to structural transformation under the condition of decoction and in the presence of the organic acidic components. These active components, existing in raw herb, might transform to a series of non-active secondary saikosaponin due to unfavourable preparation technology. So the conventional decoction-based preparation technology of Xiaochaihu granules might greatly affect its quality and therapeutic effectiveness. This study demonstrates that fingerprint-peak matching technology can not only be used for quality control of this composite formulae, but also provide some guidance for preparation technology of Xiaochaihu granules.
提出了一种利用高效液相色谱-二极管阵列检测器（HPLC-DAD）指纹峰匹配技术评价制剂工艺的方法。采用相似度和层次聚类分析（HCA）对不同厂家及本实验室的15批次小柴胡颗粒进行鉴别，并利用复方与小柴胡颗粒主要成分之一柴胡的峰型匹配，通过保留时间（RT）相对偏差和相应峰紫外光谱特征相似度等指标评价小柴胡颗粒的制剂工艺。小柴胡颗粒与柴胡之间共发现11个匹配峰。然而，在任何厂家的小柴胡颗粒中均未发现柴胡中的重要活性成分柴胡皂苷A和柴胡皂苷D。小柴胡颗粒样品11个特征峰的峰面积构成一个11×15的矩阵。HCA结果显示，小柴胡颗粒样品分为4类。同一厂家的小柴胡颗粒样品基本聚为同一类。结果表明，柴胡皂苷A和柴胡皂苷D在煎煮条件下及有机酸性成分存在时易于发生结构转化。这些存在于生药中的活性成分可能由于不利的制剂工艺而转化为一系列无活性的次生柴胡皂苷。因此，小柴胡颗粒传统的水煎制剂工艺可能会极大地影响其质量和治疗效果。本研究表明，指纹峰匹配技术不仅可用于该复方的质量控制，还可为小柴胡颗粒的制剂工艺提供一定指导。
