基于HPLC-MS^n和化学计量学的指纹图谱在毛诃子鞣质部位质量评价中的应用

Quality Evaluation of Terminalia billerica(Gaertn.) Roxb. Tannins Fraction from Different Habitats by HPLC Fingerprint Based on HPLC-MS^n and Chemometrics

目的:建立毛诃子鞣质部位HPLC指纹图谱。方法:采用Atlantic T3(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.2%冰醋酸水溶液,梯度洗脱,流速1.0 m L·min-1,进样量20μL,柱温30℃。采用相似度软件和SPSS、SIMCA软件对11批毛诃子鞣质部位的色谱数据进行化学计量学分析。结果:标定出20个共有峰。结果显示11批毛诃子鞣质部位相似度在0.832-0.973之间,只有新疆产地药材的鞣质部位的相似度在0.9以下。聚类分析将鞣质部位大致分为3类,与主成分分析结果一致。偏最小二乘判别分析找到1、13和14号峰可能是鉴别毛诃子样品最主要的色谱峰。采用HPLC-MSn方法总结出毛诃子鞣质部位中14个化合物的液质信息。结论:将毛诃子鞣质部位HPLC指纹图谱数据采用化学计量学分析方法进行分析,方法快速、简便、重复性好,可作为藏药毛诃子鞣质部位质量控制有效方法之一。

This paper was aimed to establish the HPLC fingerprint of T. Billerica（Gaertn.） Roxb. tannin fraction. The analysis was performed on Atlantic T3（250 mm × 4.6 mm, 5 μm） C18 column. The mobile phase was acetonitrile-0.2%glacial acetic acid aqueous solution with gradient elution. The flow rate was 1.0 m L·min-1. The injection size was 20 μL.The temperature was maintained at 30℃. Eleven batches of T. Billerica（Gaertn.） Roxb. tannin fraction of chromatographic data was analyzed by similarity of chromatographic data, SPSS software and SIMCA software. There were 20 common peaks in the diagram. The similarity analysis of 11 samples revealed that the similarities were between0.832 and 0.973. Only the similarity of tannin parts from Xinjiang was below 0.9. The cluster analysis classified the tannin parts into 3 types, which shared the similar results as the principal components analysis（PCA）. PLS-DA found that peak 1, 13 and 14 may be the main chromatographic peaks to identify tannins fraction. The HPLC-MSninformation of 14 compounds in T. billerica（Gaertn.） Roxb. was summarized. It was concluded that chemometrics analysis method can be used to analyze the HPLC fingerprint of T. billerica（Gaertn.） Roxb. tannin fraction. This method was rapid,simple, and reproducible. It can be used as one of the effective methods for the quality control of T. billerica（Gaertn.）Roxb. tannin fraction.