基于UPLC特征图谱和Q-Marker量值传递评价经典名方半夏白术天麻汤颗粒剂的关键生产工艺

Evaluation of key production process of Banxia Baizhu Tianma Decoction Granules based on UPLC characteristic chromatogram and Q-Marker quantitative transfer relationship

目的基于特征图谱相关性和质量标志物(quality markers,Q-Marker)转移率评价半夏白术天麻汤(Banxia Baizhu Tianma Decoction,BBTD)颗粒剂的生产环节,明确关键控制点。方法采用Acclaim;RSLC Lot Validation-120 C18色谱柱(100 mm×2.1 mm,2.2μm)进行分离,流动相为乙腈-水溶液,梯度洗脱,体积流量0.3 mL/min,检测波长235 nm,柱温30℃。以BBTD基准样品为参比,建立3批中试样品的UPLC指纹图谱,并进行相似度评价,分析Q-Marker在各生产环节的损失,评价生产工艺的合理性。结果与BBTD基准样品相比,提取液、浓缩液、干膏粉、颗粒剂中均存在对应特征峰,以10种指标性成分及其总量表征的3批BBTD中试样品关键质量属性与其基准样品基本保持一致。结论基于特征图谱和Q-Marker在各环节之间的量值传递,为经典名方BBTD制备工艺评价和质量控制提供了的理论依据。

Objective Based on the correlation of characteristic chromatogram and the transfer rate of quality markers(Q-Marker),the production process of Banxia Baizhu Tianma Decoction(半夏白术天麻汤,BBTD)Granules was evaluated,and the critical control points were identified.Methods The separation was carried out on an AcclaimTM RSLC Lot Validation-120 C18 column(100 mm×2.1 mm,2.2μm).The mobile phase was acetonitrile-aqueous solution for gradient elution,with flow rate of 0.3 mL/min,detection wavelength of 235 nm,column temperature of 30℃.Taking the reference sample of BBTD as a reference,the UPLC fingerprints of three batches of pilot samples were established,and the similarity was evaluated.The loss of Q-Marker in each production process was analyzed and the rationality of the production process was evaluated.Results Compared with the reference sample,there were corresponding characteristic peaks in extract,concentrated solution,dry paste powder and granules.The key quality attributes of three batches of pilot samples characterized by gastrodin,rutin,hesperidin,glycyrrhizin and 10 index components were basically consistent with the reference samples.Conclusion This study is based on the characteristic chromatogram and the value transfer of Q-Marker between each link,which provides a theoretical basis for the preparation process evaluation and quality control of classical prescriptions BBTD.