摘要
目的:建立经典名方清肺汤基准样品的特征图谱及指标性成分含量测定方法,阐明清肺汤的关键质量属性.方法:制备 15 批清肺汤基准样品,建立高效液相色谱法(HPLC)特征图谱方法,并进行特征峰归属和相似度分析;以苦杏仁苷、栀子苷、橙皮苷、黄芩苷、汉黄芩苷、黄芩素、甘草酸为指标性成分建立清肺汤多成分含量测定方法,对指标成分的含量和转移率进行分析研究,以均值的 70%～130%为界限设定各质量控制指标的量值波动范围.结果:15 批清肺汤基准样品的HPLC特征图谱相似度为 0.986～0.999,共 16 个特征峰,经对照品指认出 12个特征峰,分别为京尼平龙胆二糖苷、苦杏仁苷、栀子苷、橙皮苷、黄芩苷、去甲汉黄芩苷、千层纸素A-7-O-β-D-葡萄糖醛酸苷、汉黄芩苷、黄芩素、汉黄芩素、五味子醇甲、千层纸素A;指标性成分从饮片到物质基准的转移率分别为苦杏仁苷 24.35%～33.13%、栀子苷 36.78%～49.55%、橙皮苷 23.11%～35.92%、黄芩苷 60.62%～74.15%、汉黄芩苷 61.81%～76.90%、黄芩素 9.21%～15.77%、甘草酸 10.35%～18.46%.结论:采用特征图谱结合多指标成分含量测定对清肺汤基准样品的量值传递规律进行研究,该方法重现性好、简便、准确、稳定,为经典名方清肺汤基准样品的质量控制及复方制剂的开发提供参考.
Abstract
Objective:To establish the characteristic chromatogram and index component content determination method for Qingfei Decoction benchmark samples,and clarify the key quality attributes of Qingfei Decoction.Methods:Fifteen batches of Qingfei Decoction benchmark samples were prepared.The HPLC characteristic chromatogram method was established,followed by characteristic peak attribution and similarity analysis.A multi-component content determination method for Qingfei Decoction was established using amygdalin,geniposide,hesperidin,baicalin,wogonoside,baicalein,and glycyrrhizic acid as indicator components.The content and transfer rates of the indicator components were analyzed,and 70%-130%of the average mass was regarded as the limit for the quantity value range of quality control indexes.Results:The similarity of the 15 batches of Qingfei Decoction benchmark samples was 0.986-0.999,with a total of 16 characteristic peaks.Twelve characteristic peaks were identified using reference substances:genipin 1-gentiobioside,amygdalin,geniposide,hesperidin,baicalin,norwogonoside,oroxylin A-7-O-β-D-glucuronide,wogonoside,baicalein,wogonin,schisandrin,and oroxylin A.The transfer rates from the decoction pieces to the benchmark samples were 24.35%-33.13%for amygdalin,36.78%-49.55%for geniposide,23.11%-35.92%for hesperidin,60.62%-74.15%for baicalin,61.81%-76.90%for wogonoside,9.21%-15.77%for baicalein,and 10.35%-18.46%for glycyrrhizic acid.Conclusion:The characteristic chromatogram combined with the content determination of multiple index components was used to study the value transfer law of the benchmark samples of Qingfei Decoction.The method showed good reproducibility,simplicity,accuracy,and stability,providing a reference for the quality control of the classical prescription Qingfei Decoction benchmark samples and the development of Qingfei Decoction compound formulations.
基金项目
河北省自然科学基金项目(H2022329003)
河北省药品监督管理局科技计划项目(2022ZC1019)
维普
万方数据