[关键词]
[摘要]
目的 建立藏药毛诃子药材HPLC指纹图谱,测定毛诃子中没食子酸、柯里拉京、鞣花酸和没食子酸甲酯量,为毛诃子药材质量控制提供依据。方法 采用Atlantic T3(250 mm×4.6 mm,5 μm)色谱柱,乙腈-0.2%冰醋酸水溶液为流动相,梯度洗脱,体积流量1.0 mL/min,进样量20 μL,柱温30℃。建立11批毛诃子药材HPLC指纹图谱共有模式,并采用化学计量学分析方法分析隐藏信息。采用HPLC-MSn对毛诃子药材色谱峰进行指认,并对特征峰进行定量分析。结果 得到毛诃子HPLC指纹图谱,标示出21个共有峰,相似度均在0.9以上。采用HPLC-MSn方法指认了18个化合物。主成分分析和聚类分析将样品大致分为3类。并结合偏最小二乘判别分析方法发现区分毛诃子样品的5个标志性化合物,其中指认出12号峰为诃子鞣酸。定量分析条件通过方法学验证,平均加样回收率在97.24%~98.58%。结论 对HPLC指纹图谱和主要成分量同时进行分析,方法快速、简便、重复性好,可作为藏药毛诃子质量控制有效方法之一。
[Key word]
[Abstract]
Objective To establish the HPLC fingerprint and to determin gallic acid, methyl gallate, corilagin, and ellagic acid in Terminalia billerica, in order to provide the scientific foundation for quality control of T. billerica. Methods The analysis was performed on Atlantic T3 (250 mm×4.6 mm, 5 μm) C18 column, mobile phase was acetonitrile-0.2% glacial acetic acid aqueous solution with gradient elution, flow rate was 1.0 mL/min, injection size was 20 μL column, and temperature was maintained at 30℃. The common mode of T. billerica HPLC fingerprint was established, the hidden information was analyzed in the fingerprint by Chemometrics, and the components in T. billerica by HPLC-MSn and quantitative analysis characteristic peaks were identified. Results There were 21 common peaks in the diagram and the similarity of the fingerprints was over 0.9 in all 11 batches. The information of the 18 common peaks in T. billerica was summarized by HPLC-MSn technology. The samples were broadly divided into three kinds by principal component analysis and clustering analysis. The five key compounds were verified by partial least squares discriminant analysis method in quantitative analysis, and identified that the No.12 peak was chabulagic acid, and the average recoveries were in the range of 97.24%-98.58%. Conclusion The HPLC fingerprint method and content determination method are reliable, accurate, rapid, simple, and reproducible, and this study could control the quality of T. billerica.
[中图分类号]
[基金项目]