[关键词]
[摘要]
目的 建立旋覆代赭汤(Xuanfu Daizhe Decoction,XDD)中9种酚酸类成分一测多评(quantitative analysis of multi-components by single marker,QAMS)定量测定方法,研究酚酸类成分的传递规律,结合基准关联度,分析配伍的影响,并探究“去渣再煎”的影响。方法 制备15批XDD基准样品,以绿原酸为内标物,确定其他8种成分的相对校正因子(fs/i)并计算含量,同时采用外标法测定,比较两者结果差异,计算饮片-水煎液-基准样品的转移率,分析传递规律;制备不同配伍样品,以9种酚酸类成分转移率和指纹图谱相似度为评价指标,计算基准关联度;制备不同煎煮条件样品,检测9种酚酸类成分的转移率。结果 QAMS法定量测定结果与外标法无显著差异。新绿原酸、绿原酸、隐绿原酸、咖啡酸、1,3-二咖啡酰奎宁酸、异绿原酸B、异绿原酸A、1,5-二咖啡酰奎宁酸、异绿原酸C的平均转移率分别为147.34%、42.60%、321.53%、131.49%、419.76%、172.93%、18.47%、25.06%、74.68%,酚酸类成分发生降解与异构化可能是部分成分转移率大于100%的主要原因;配伍、煎煮时间、浓缩对9种酚酸类成分的传递均有影响,其中旋覆花与半夏配伍后各指标成分和指纹图谱相似度的基准关联度均大于90%,而“去渣再煎”可以进一步促进酚酸类成分的降解与异构化。结论 建立的QAMS法方便、稳定,初步明确从饮片到XDD基准样品中酚酸类有效成分群之间的变化、量值传递规律和可能的影响因素,为XDD的质量控制和制剂开发提供科学依据。
[Key word]
[Abstract]
Objective To establish QAMS for the determination of nine phenolic acids in Xuanfu Daizhe Decoction (XDD, 旋覆代赭汤), study the transfer rule of phenolic acids, analyze the influence of compatibility combined with the standard relation, and explore the influence of “remove the residue and concentrate again”. Methods A total of 15 batches of XDD samples were prepared, chlorogenic acid was used as the internal standard, the relative correction factor (fs/i) of other eight components were determined and the content was calculated, and the external standard method was used to determine the difference between the two results, and the transfer rate of decoction slices, water decoction and reference sample was calculated and the transfer law was analyzed. Different compatible samples were prepared, the transfer rate of nine phenolic acids and the similarity of fingerprint were used as evaluation indexes, and the standard relation was calculated. The transfer rates of nine phenolic acids were determined by preparing samples under different cooking conditions. Results There was no significant difference between QAMS method and external standard method. The average transfer rates of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, 1,3-dicaffeoyl quinic acid, isochlorogenic acid B, isochlorogenic acid A, 1,5-dicaffeoyl quinic acid and isochlorogenic acid C were 147.34%, 42.60%, 321.53%, 131.49%, 419.76%, 172.93%, 18.47%, 25.06% and 74.68%, respectively. The degradation and isomerization of phenolic acids may be the main reason that the transfer rate of some components is greater than 100%. Compatibility, decocting time and concentration all had effects on the transfer of nine phenolic acids. The standard relation of each index component and fingerprint similarity between convolution flower and pinellia were all greater than 90%, and “de-slagging and re-decocting” could further promote the degradation and isomerization of phenolic acids. Conclusion The established QAMS method is convenient and stable, and the changes of phenolic acid active component groups from XDD from decoction pieces to reference samples, the transfer rule of quantity value and possible influencing factors are preliminatively identified, which provides a scientific basis for the quality control and preparation development of XDD.
[中图分类号]
R283.6
[基金项目]
江苏省自然科学基金青年项目(BK20180265);江苏省中药骨干人才高级研修项目;江苏省中医药科技发展计划项目(QN202420);苏州科技计划项目(SKY2022076);苏州市应用基础研究科技创新项目(SYWD2024261);昆山市社会发展项目(KS2234、KS2327)