经典名方吴茱萸汤基准样品特征图谱及含量测定研究

Study on characteristic chromatogram and content determination of Wuzhuyu Decoction reference sample

以特征图谱、指标性成分含量及干膏率为指标,探索吴茱萸汤基准样品的关键质量属性,考察药材-饮片-基准样品的量值传递关系,初步拟定基准样品质量标准。建立15批吴茱萸汤HPLC特征图谱,进行相似度分析,标定共有峰并进行药材归属,并对吴茱萸汤中柠檬苦素、吴茱萸碱、吴茱萸次碱、人参皂苷Rb进行定量检测。结合干膏率、特征图谱相似度及指标性成分含量的转移率进行量值传递的研究。吴茱萸汤基准样品对应实物共标定18个共有峰,特征图谱相似度均大于0.9,吴茱萸、人参、生姜、大枣分别贡献9、5、8、2个色谱峰;不同批次基准样品对应实物的指标性成分含量和药材-饮片、饮片-基准样品转移率如下:柠檬苦素质量分数为0.16%~0.51%,转移率分别为83.66%~115.60%、38.54%~54.58%;吴茱萸碱质量分数为0.01%~0.11%,转移率分别为80.80%~116.15%、3.23%~12.93%;吴茱萸次碱质量分数为0.01%~0.05%,转移率分别为84.33%~134.53%、5.72%~21.24%;人参皂苷Rb质量分数为0.06%~0.11%,转移率分别为90.00%~96.92%、32.45%~67.24%;全方的干膏率为22.58%~29.89%。该实验采用特征图谱、指标性成分含量测定及干膏率相结合的模式,对经典名方吴茱萸汤基准样品的量值传递过程进行分析,初步建立了科学稳定的基准样品质量评价方法,为经典名方吴茱萸汤的后续开发及相关制剂的质量控制提供依据。

In this study, the critical quality attributes of Wuzhuyu Decoction reference sample were explored by using characteristic chromatogram, index component content and dry extract rate as indexes.The dissemination relationship of quantity value between medicinal materials-decoction pieces-reference sample was investigated to preliminarily formulate the quality standard of the reference sample.The characteristic chromatogram of 15 batches of Wuzhuyu Decoction was established by high performance liquid chromatography(HPLC) and the similarity analysis was conducted.Common peaks were demarcated and assigned to medicinal materials.Moreover, quantitative determination of limonin, evodiamine, rutaecarpine and ginsenoside Rbof Wuzhuyu Decoction were performed.The dissemination of quantity value was explored combined with dry extract rate, similarity of characteristic chromatogram and transfer rate of index component content.A total of 18 common peaks were identified in the corresponding materials of Wuzhuyu Decoction reference sample, with the similarity of characteristic chromatogram greater than 0.9, and Fructus Evodiae, Radix Ginseng, Rhizoma Zingiberis Recens and Fructus Jujubae contributed 9, 5, 8 and 2 chromatographic peaks, respectively.The index component content of corresponding materials and the transfer rates of medicinal materials-decoction pieces and decoction pieces-reference sample of different batches of Wuzhuyu Decoction reference sample were as follows: the content of limonin was 0.16%-0.51%, and the transfer rates were 83.66%-115.60% and 38.54%-54.58%, respectively;the content of evodiamine was 0.01%-0.11%, the transfer rated were 80.80%-116.15% and 3.23%-12.93%, respectively;the content of rutaecarpine was 0.01%-0.05%, the transfer rates were 84.33%-134.53% and 5.72%-21.24%, respectively;the content of ginsenoside Rbwas 0.06%-0.11%, and the transfer rates were 90.00%-96.92% and 32.45%-67.24%, respectively.The dry extract rate of the whole prescription was 22.58%-29.89%.In this experiment, the dissemination of quantity value of Wuzhuyu Decoction reference sample was analyzed by the combination of characteristic chromatogram, index component content and dry extract rate.A scientific and stable quality evaluation method of the reference sample was preliminarily established, which provided basis for the subsequent development of Wuzhuyu Decoction and the quality control of related preparations.