加味柴胡疏肝散基准样品HPLC指纹图谱及关键质量属性量值传递规律研究

HPLC fingerprint of Modified Chaihu Shugan Powder benchmark sample and quantity transfer law of key quality attributes

目的建立加味柴胡疏肝散(Modified Chaihu Shugan Powder,MCSP)基准样品HPLC指纹图谱及多成分含量测定的方法,结合化学模式分析,探究关键质量属性的传递规律。方法制备40批MCSP样品,利用HPLC法,以乙腈-0.2%磷酸水溶液为流动相,采用“中药色谱指纹图谱相似度评价软件(2012年版)”计算其相似度,结合化学计量法分析多产地多批次MCSP基准样品,结合指标性成分含量以及转移率,进行量值传递分析及整体质量研究。结果建立的40批MCSP基准样品相似度大于0.90,指纹图谱相似度良好,29个共有峰中指认出其中13个色谱峰,所建立的多成分含量测定方法稳定可靠。芍药内酯苷、芍药苷、阿魏酸、芸香柚皮苷、柚皮苷、橙皮苷、橙皮素、新橙皮苷、去氢木香内酯、柴胡皂苷A的平均转移率分别为29.96%、22.08%、32.98%、22.42%、33.26%、15.50%、34.23%、56.94%、8.66%、8.69%。结论采用指纹图谱结合多指标成分含量测定及转移率等评价指标对MCSP基准样品进行了量值传递综合考察,初步构建MCSP全过程质量控制体系,为制剂开发及MCSP的进一步研究提供参考。

Objective To establish the fingerprint and multi-component content determination method of Modified Chaihu Shugan Powder(加味柴胡疏肝散,MCSP)benchmark sample,and explore the transmission law of key quality attributes by combining chemical pattern analysis.Methods A total of 40 batches of MCSP samples were prepared by HPLC method with acetonitrile-0.2%phosphate water as mobile phase,and the similarity was calculated by using the Chinese Medicine Chromatographic Fingerprint Similarity Evaluation Software(2012 edition),combined with stoichiometric analysis,multiple batches of MCSP samples from multiple origins were analyzed,and the value transfer analysis and overall quality study were carried out in combination with the index component content and transfer rate.Results The benchmark similarity of 40 batches of MCSP substances was greater than 0.90,and the similarity of the characteristic map was good,with a total of 29 common peaks,of which 13 peaks were identified,and the established multi-component content determination method was stable and reliable.The average transfer rates of albiflorin,paeoniflorin,ferulic acid,narirutin,naringin,hesperidin,hesperetin,neohesperidin,dehydrocostuslactone,saikosaponin A were 29.96%,22.08%,32.98%,22.42%,33.26%,15.50%,34.23%,56.94%,8.66%and 8.69%,respectively.Conclusion The characteristic map was used to combine the evaluation indicators such as multi-index component content determination and transfer rate to comprehensively investigate the measurement value transfer of MCSP benchmark samples,and the quality control system of the whole process of MCSP was preliminarily constructed,which provided reference for the development of preparations and further research of MCSP.