基于UPLC-Q-TOF MS技术的血栓心脉宁片成分分析
Comprehensive Component Screening of Xueshuan Xinmaining Tablet Based on UPLC-Q-TOF MS
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摘要: 为全面了解中药大品种血栓心脉宁片（XXT）化学成分，采用超高效液相色谱-四极杆飞行时间串联质谱联用技术（UPLC-Q-TOF MS）测定该复方制剂的小分子成分（100~1 500 u），通过UNIFI天然产物分析平台，比对各成分的精确分子质量、保留时间及质谱碎片离子信息，分析鉴定各化合物结构。结果表明，在XXT中共鉴定出187种化学成分，包括三萜皂苷类、菲醌类、蟾蜍甾二烯类和甾体类及其他结构类型的化合物。血栓心脉宁片富含小分子化学成分且结构类型多样，是其发挥抗血瘀活性及多靶点作用机制的物质基础。该研究可为阐明XXT的药效物质基础和提升质量控制标准提供数据参考。Abstract: For comprehensively understanding of the chemical composition in Xueshuan Xinmaining Tablet（XXT）, ultra high performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF MS) was developed. The automated data processing software UNIFI was selected to perform the screening analysis on the structural characteristics and MS fragmentation behavior, especially for characteristic fragments. Separation was performed on a Waters ACQUITY UPLC BEH C18 column (100 mm×2.1 mm×1.7 μm) at 40 ℃. The mobile phase was consisted of 0.1% formic acid aqueous solution (A) and 0.1% formic acid in acetonitrile (B) with the flow rate of 0.4 mL/min. The data were collected with Masslynx V4.1 workstation. The MS raw data were processed using the streamlined workflow of UNIFI software to quickly identify the chemical components that met the match criteria with the in-house Traditional Medicine Library and the self-built database. The self-built database of compounds, such as saponins, flavonoids, volatile oil, amino acids and so on, was established by searching online databases such as China Journals of Full-Text Database (CNKI), PubMed, Medline, Web of Science and ChemSpider. By comparing the exact molecular mass, retention time, and mass spectrometry fragment ion information of each component, a total of 187 chemical constituents are identified, including triterpenoid saponins, phenanthrenes, oxadienes, steroids and other structural types of compound. This method is rapid and comprehensive for analysis of the chemical constituents of complicated herbal extracts. XXT is rich in small chemical components with various structural types. The study offers the pharmacodynamic basis for antithrombus effect and multi-target mechanism of XXT.
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