[关键词]
[摘要]
目的 为更加全面、系统、快速地表征芪参益气滴丸有效化学成分谱,对芪参益气滴丸中主要化学成分进行快速识别鉴定和归属分类。方法 采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q-Orbitrap HRMS)技术, ACQUITY UPLC® BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),以乙腈(A)-0.1%甲酸水(B)为流动相进行梯度洗脱,以实现化合物的前期分离;通过先进的Q-Orbitrap MS技术捕捉未知成分的精确相对分子质量及多级碎片离子信息,同时与对照品的保留时间和质谱数据信息进行匹配,并结合相关文献以及Chemical Book、Mass Bank等数据库最终实现对中药中复杂成分的快速准确识别。结果 共鉴定出53种化学成分,其中包括有机酸类14种、黄酮类10种、醌类10种、皂苷类2种、氨基酸类7种及其他类10种。结论 本法可快速、准确地识别芪参益气滴丸中主要化学成分,同时为其进一步的药效物质基础、质量控制及临床合理应用等研究奠定了科学的前期基础。
[Key word]
[Abstract]
Objective To recognize the chemical profile of Qishen Yiqi Dropping Pills (QYDP) comprehensively, systematically and rapidly; ultra high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was employed to identify the main chemical composition of this preparation. Methods A gradient elution for separation was achieved through ACQUITY UPLC® BEH C18 column (100 mm×2.1 mm, 1.7 μm) with acetonitrile-water (containing 0.1% formic acid) as the mobile phase. Then, the novel Q-Orbitrap MS technology was employed to detect the information of accurate mass and multistage fragment ions. Chemical constituents were characterized by comparing their relative retention time and mass data with that of the reference substance, meanwhile the reference literature, Mass Bank database, and Chemical Book network database were also consulted. Results A total of 53 ingredients were finally identified in this study, including 14 organic acids, 10 flavones, 10 authraquinones, 2 saponins, 7 amino acids, and 10 others. Conclusion An efficient method was established in this work to identify the main chemical ingredients of QYDP rapidly and accurately; Meanwhile, this research will lay a scientific foundation for the further research on pharmacodynamic material basis, quality control, and clinical application of this medicine.
[中图分类号]
[基金项目]
郑州大学第一附属医院创新基金项目(2017)