[关键词]
[摘要]
目的 建立升陷汤标准煎液的物理指纹图谱及6种指标成分(毛蕊异黄酮葡萄糖苷、刺芒柄花苷、毛蕊异黄酮、芒柄花黄素、芒果苷、异阿魏酸)含量测定方法,为其质量评价奠定基础。方法 基于遵古理念制备15批升陷汤标准煎液,以溶解性固体总量、pH值、密度、动力黏度、电导率、表面张力、折光率及固含量8个物理参数构建升陷汤标准煎液物理指纹图谱;采用相似度评价、主成分分析(principal component analysis,PCA)及层次聚类分析(hierarchical cluster analysis,HCA)对物理指纹图谱进行评价及异常样品判断。以HPLC法测定毛蕊异黄酮葡萄糖苷、刺芒柄花苷、毛蕊异黄酮、芒柄花黄素、芒果苷、异阿魏酸6种指标成分含量,结合多元统计分析方法进行分析。结果 15批升陷汤标准煎液的物理指纹图谱存在差异,主要体现在溶解性固体总量、动力黏度及电导率3个指标上;相似度分析与PCA结果显示,15批标准煎液相似度均大于0.9,15批标准煎液聚为2类,A1、A2、A3、A8、A12、A13、A15聚为一类,其余标准煎液聚为一类。由DMod X控制图监测显示,15批标准煎液均为正常样品;15批标准煎液中6种指标成分质量浓度分别为毛蕊异黄酮葡萄糖苷4.81~6.30 μg/mL、刺芒柄花苷1.50~1.78 μg/mL、毛蕊异黄酮3.50~4.65 μg/mL、芒柄花黄素1.33~1.63 μg/mL、芒果苷68.33~75.23 μg/mL、异阿魏酸3.50~5.65 μg/mL,15批标准煎液指标成分含量HCA结果与物理指纹图谱HCA结果一致。结论 构建的升陷汤标准煎液物理指纹图谱与指标成分含量测定方法,可用于其一致性评价、质量控制及其煎煮全过程的动态监控。
[Key word]
[Abstract]
Objective To establish the physical fingerprint of the standard decoction of Shengxian Decoction (升陷汤), and to determine the contents of six index components (calycosin-7-O-β-D-glucoside, ononin, calycosin, formononetin, mangiferin and isoferulic acid), lay a foundation for its quality evaluation. Methods Fifteen batches of standard decoction of Shengxian Decoction were porepared based on the concept of abiding by the ancient times. The physical fingerprint of the standard decoction of Shengxian Decoction was constructed from eight physical parameters: Total dissolved solids (TDS), hydrogen ion concentration (pH), density (ρ), dynamic viscosity (μ), conductivity (σ), surface tension (γ), refractive index (n), and solid content (SC). The similarity evaluation, principal component analysis (PCA) and hierarchical cluster analysis (HCA) were used to evaluate the physical fingerprint and judge the abnormal samples. The content of six index components of calycosin-7-O-β-D-glucoside, ononin, calycosin, formononetin, mangiferin and isoferulic acid were determined by HPLC. Combined with multivariate statistical analysis method. Results The physical fingerprints of 15 batches of standard decoction of Shengxian Decoction were different, mainly reflected in three indicators: TDS, μ and σ. The results of similarity analysis and PCA showed that the similarity of 15 batches of standard decoction was greater than 0.9, they were grouped into two categories, A1, A2, A3, A8, A12, A13 and A15 into one category, and the rest of the standard decoctions were grouped into one category. The monitoring of DMod X control chart showed that 15 batches of standard decoctions are all normal samples. The mass concentrations of six index components in 15 batches of standard decoctions were respectively 4.81—6.30 μg/mL of calycosin-7-O-β-D-glucoside, 1.50—1.78 μg/mL of ononin, 3.50—4.65 μg/mL of calycosin, 1.33—1.63 μg/mL of formononetin, 68.33—75.23 μg/mL of mangiferin, 3.50—5.65 μg/mL of isoferulic acid. The HCA results of 15 batches of standard decoctions were consistent with those of physical fingerprint. Conclusion The physical fingerprint and index component content determination method of Shengxian Decoction can be used for consistency evaluation, quality control and dynamic monitoring of the whole decoction process.
[中图分类号]
R283.6
[基金项目]
吉林省科技发展计划项目(20180201089YY);重大疫情防治中药方剂储备库建设项目(吉中医药发[2021]11号);校企合作项目(2018-2200-02-000490)