经典名方真武汤的物质基准关键质量属性

Key Quality Attributes of Substance Benchmark of Famous Classical Formula ZhenWu Tang

目的:建立真武汤物质基准的特征图谱及多指标成分含量测定方法,并阐明真武汤的关键质量属性,以期为经典名方真武汤物质基准及制剂的质量评价研究提供参考。方法:使用不同批次饮片制备15批真武汤物质基准冻干粉,采用高效液相色谱法(HPLC)建立真武汤特征图谱,并进行特征峰归属和相似度分析;以芍药苷、6-姜辣素为指标性成分建立真武汤多成分含量测定方法,以均值的70%~130%为界限设定各质量控制指标的量值范围,并对15批真武汤物质基准进行量值传递分析。结果:15批真武汤物质基准的特征图谱共有11个特征峰,指认出没食子酸、5-羟甲基糠醛、(+)-儿茶素、芍药苷、苯甲酰芍药苷、6-姜辣素、8-姜酚7个色谱峰,相似度均大于0.99;15批真武汤物质基准中指标性成分芍药苷质量分数20.01~25.35 mg·g^(-1),转移率49.77%~69.84%;6-姜辣素质量分数1.65~2.57 mg·g^(-1),转移率30.11%~58.96%;出粉率3.21%~4.57%。结论:建立的真武汤物质基准HPLC特征图谱及多成分含量测定方法简单可行,重复性、稳定性良好,可为经典名方真武汤物质基准及制剂关键化学属性的质量评价提供参考。

Objective:To establish the characteristic chromatogram and the content determination method of index components in substance benchmark of famous classical formula ZhenWu Tang,so as to clarify the key quality attributes of ZhenWu Tang and provide reference for studying the quality evaluation of ZhenWu Tang substance benchmark and preparations.Methods:A total of 15 batches of freeze-dried powder of ZhenWu Tang substance benchmark were prepared with different batches of decoction pieces.The HPLC characteristic chromatogram of ZhenWu Tang was established,and the attributes and similarities of the characteristic peaks were analyzed.With paeoniflorin and 6-gingerol as index components,the muti-index content determination method was constructed,and the 70%-130%of the mass average was regarded as the limit for the quantity value range of quality control indexes.In addition,the quantity value transfer of the 15 batches of ZhenWu Tang substance benchmark was analyzed.Results:There were 11 characteristic peaks corresponding to the characteristic chromatogram of the 15 batches of ZhenWu Tang substance benchmark,and seven chromatographic peaks[gallic acid,5-hydroxymethylfurfural,(+)-catechin,paeoniflorin,benzoyl paeoniflorin,6-gingerol and 8-gingerol]were identified,with the similarity all more than 0.99.The content and transfer rate of index components in the 15 batches of substance benchmarks were as follows:paeoniflorin content 20.01-25.35 mg·g^(-1) and transfer rate 49.77%-69.84%;6-gingerol content 1.65-2.57 mg·g^(-1) and transfer rate 30.11%-58.96%;the powder yield rate was 3.21%-4.57%.Conclusion:The established characteristic chromatogram and content determination methods of ZhenWu Tang substance benchmark in this study were simple,feasible,reproducible and stable,and could provide reference for further research on the key chemical properties of ZhenWu Tang substance benchmark and preparations.