基于HPLC-Q-TOF-MS/MS技术快速分析肠炎宁片中主要化学成分

Main chemical constituents of Changyanning Tablets based on HPLC-Q-TOF-MS/MS

目的为更加全面、系统、快速地表征肠炎宁片中的化学物质基础,采用高效液相色谱-四级杆飞行时间高分辨质谱(HPLC-Q-TOF-MS/MS)技术对肠炎宁片中化学成分进行快速识别和归属分类。方法采用AgilentZORBAXEclipse XDB-C_(18)色谱柱(250 mm×4.6 mm,5μm),以甲醇(A)-0.05%乙酸水(B)为流动相进行梯度洗脱,质谱负离子模式监测及二级质谱扫描进行数据采集。通过高分辨质谱数据,结合Pubmed、Hmdb、Massbank数据库、参考相关文献以及对照品比对,鉴定肠炎宁片的主要化学成分。结果从肠炎宁片中共鉴定了51个化学成分,包括2个苯丙素类、8个环烯醚萜类、12个黄酮类、4个鞣质类、23个有机酸类及2个其他类成分。结论全面地阐述了肠炎宁片中的化学物质基础,为提升肠炎宁片质量评价体系和阐明其药效物质提供了依据。

Objective To study the chemical constituents of Changyanning Tablets, a high performance liquid chromatography-quadrupole time of flight mass spectrometry(HPLC-Q-TOF-MS/MS) was established to recognize and classify the ingredients accurately and rapidly. Methods Agilent ZORBAX Eclipse XDB-C18 chromatographic column(250 mm × 4.6 mm, 5 μm) was employed and the separation was performed with the mobile phase consisting of methanol-0.05% acetic acid aqueous solution. The information of accurate mass and multistage fragment ions were obtained by the monitored simultaneously for positive and negative ions. The main chemical constituents of Changyanning Tablets were identified by high resolution mass spectrometry data, combining with Pubmed, Hmdb, Massbank network database, reference literature and comparing the reference. Results Fifty-one chemical components were finally identified in this study, including two phenylpropanoids, eight iridoids, 12 flavonoids, four tannins, 23 organic acids, and two other classes. Conclusion This study comprehensively studies the material basis in Changyanning Tablets, which provides a basis for improving the quality evaluation system of Changyanning Tablets and lays the foundation for elucidating the active components mechanism.