川芎饮片标准汤剂的质量分析

目的:制备川芎饮片标准汤剂并对其进行质量分析。方法:参照标准汤剂的要求,制备来自3个产地共15批川芎饮片标准汤剂;建立其HPLC指纹图谱,采用聚类分析进行质量分析;建立其指纹图谱共有模式下4种指标成分(阿魏酸,洋川芎内酯Ⅰ,洋川芎内酯A和藁本内酯)的HPLC含量测定方法;计算各批次样品中指标成分转移率、出膏率,并测定样品的pH。结果:对15批川芎饮片标准汤剂采用"中药色谱指纹图谱相似度评价系统"(2012A版)进行指纹图谱分析,确定了22个共有峰,其相似度均0.92;定性指认出其中11,13,17,18,19,20号峰,分别为阿魏酸,洋川芎内酯Ⅰ,洋川芎内酯A,正丁基苯酞,阿魏酸松柏酯,藁本内酯;通过聚类分析可将3个产地的川芎饮片标准汤剂质量概貌进行区分,说明不同产地的川芎存在质量差异,但同一产地不同批次质量较为稳定。15批川芎饮片标准汤剂共有模式下4种主要成分分别为阿魏酸,洋川芎内酯Ⅰ,洋川芎内酯A和藁本内酯;以洋川芎内酯A(0.176 3~0.249 8 g·L~(-1))和洋川芎内酯Ⅰ(0.065 2~0.103 4 g·L~(-1))在标准汤剂中含量较高,藁本内酯(0.040 0~0.089 8 g·L~(-1))次之,阿魏酸(0.022 0~0.042 3 g·L~(-1))最低,4个成分的转移率依次为6.63%~11.82%,33.32%~55.98%,1.26%~3.73%,16.39%~33.05%;15批川芎饮片标准汤剂的干膏得率12.69%~19.78%,pH 4.54~4.82。结论:该研究建立了各产地多批次川芎饮片标准汤剂的指纹图谱和多成分含量测定方法,适用于川芎饮片标准汤剂的质量控制。

Quality Analysis of Standard Decoction of Chuanxiong Rhizoma

Objective: To prepare standard decoction of Chuanxiong Rhizoma and conduct its quality analysis.Method: According to the requirements of standard decoction,15 batches of standard decoction of Chuanxiong Rhizoma from three producing areas were prepared,the HPLC fingerprint was established and the quality analysis was carried out by cluster analysis;under common pattern of fingerprint,the simultaneous determination of four index components (ferulic acid,senkyunolide I,senkyunolide A and ligustilide) was established by HPLC.The transfer rates of main components,dry extract yield,pH value of samples were measured.Result: A total of 15 batches of standard decoctions of Chuanxiong Rhizoma were fingerprinted by Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine (edition of 2012A).Twenty-two common peaks were identified,and their similarities were all greater than 0.92,and peak 11,13,17,18,19 and 20 were identified qualitatively as ferulic acid,senkyunolide I,senkyunolide A,n-butylphthalide,coniferyl ferulate and ligustilide,respectively.The quality overview of standard decoction of Chuanxiong Rhizoma from three producing areas could be distinguished through cluster analysis,which showed that there were differences in quality of Chuanxiong Rhizoma from different producing areas,but the quality was relatively stable in different batches of samples from the same origin.Under common pattern,there were four major components in 15 batches of standard decoction of Chuanxiong Rhizoma,including ferulic acid,senkyunolide I,senkyunolide A and ligustilide.Contents of senkyunolide A (0.176 3-0.249 8 g·L^-1) and senkyunolide I (0.065 2-0.103 4 g·L^-1) was high in the standard decoction,content of ligustilide (0.040 0-0.089 8 g·L^-1) followed,and content of ferulic acid (0.022 0-0.042 3 g·L^-1) was the lowest,transfer rates of the above four components were 6.63%-11.82%,33.32%-55.98%,1.26%-3.73% and 16.39%-33.05%,respectively.Dry extract yield of the standard decoction was 12.69% to 19.78%,and the pH was 4.54 to 4.82.Conclusion: This study establishes the fingerprint and multi-component determination methods of standard decoctions of Chuanxiong Rhizoma from various producing areas,which is suitable for quality control of this standard decoction.