[关键词]
[摘要]
目的 制备15批川芎饮片标准汤剂,建立其HPLC指纹图谱和物理指纹图谱并对其进行质量评价。方法 按《中药配方颗粒质量控制与标准制定技术要求(征求意见稿)》中标准汤剂制备条件,制备15批川芎饮片标准汤剂,采用HPLC,流动相为0.6%磷酸水溶液-乙腈,进行梯度洗脱,柱温30 ℃,体积流量1.0 mL/min,检测波长324 nm,建立川芎饮片标准汤剂的HPLC指纹图谱;并建立由9个2级指标(相对均齐度指数、颗粒间空隙率、卡尔指数、松密度、振实密度、干燥失重、吸湿性、豪斯纳比、休止角)构成的物理指纹图谱。结果 HPLC对照指纹图谱中主要共有峰有13个,确认3个,分别为绿原酸、咖啡酸和阿魏酸。以阿魏酸为参照峰,分析了各共有峰的相对保留时间和相对峰面积,并规定了各共有峰相对保留时间和相对峰面积的限度。建立了HPLC及物理指纹图谱,并规定其相似度均不应低于0.9。结论 建立的川芎饮片标准汤剂的HPLC和物理指纹图谱可作为合理稳定的质量评价指标,为川芎配方颗粒的研制及质量控制提供参考。
[Key word]
[Abstract]
Objective To prepare 15 batches of Chuanxiong Rhizoma standard decoction, and establish HPLC fingerprint and physical fingerprint for quality evaluation. Methods Fifteen batches of Chuanxiong Rhizoma standard decoction were prepared according to preparation conditions of the traditional Chinese medicine (TCM) standard decoction in "Technical Requirements for Quality Control and Standard Formulation of Prescription Granules of TCM (draft for soliciting opinions)". The mobile phase of HPLC consisted of 0.6% aqueous solution of phosphoric acid and acetonitrile with gradient elution, column temperature of that was 30℃, flow rate of that was 1.0 mL/min and detection wavelength of that was 324 nm. Physical fingerprint that consisted of nine secondary indexes (relative homogeneity index, intergranular porosity, Karl index, loose density, vibrating density, dry weight loss, hygroscopicity, Hausner ratio, and angle of repose) was established. Results There were 13 common peaks in the HPLC control fingerprint, and three of them were identified as chlorogenic acid, caffeic acid, and ferulic acid respectively. Taking ferulic acid as a reference peak, the relative retention time and relative peak area of each co-owned peak were analyzed, and the limits of relative retention time and relative peak area of each co-owned peak were specified. The HPLC and physical fingerprint were established, and the similarity should greater than 0.9. Conclusion The HPLC and physical fingerprint of the Chuanxiong Rhizoma standard decoction can be used as reasonable and stable index to evaluate the quality of Chuanxiong Rhizoma standard decoction. Which provides a reference for the preparation and quality control of Chuanxiong Rhizoma dispensing granule.
[中图分类号]
[基金项目]
四川省科技厅2018年科技项目(2018TJPT0049,2018ZR0107);四川千人计划支持项目(2013332);成都大学教改项目(cdjgy2017010)