高效液相色谱-高分辨质谱法鉴定拉萨大黄化学成分

建立了高效液相色谱-高分辨质谱法分析鉴定拉萨大黄化学成分。选用Agilent Zorbax SB-C18柱（150 mm×4.6 mm×5 μm），以乙腈和水为流动相进行梯度洗脱，流速0.5 mL/min；采用电喷雾离子源，在正、负离子模式下对拉萨大黄提取物进行一级和多级全扫描质谱分析。综合分析化合物的色谱和质谱行为，并结合对照品、文献和数据库等相关数据鉴定化合物。在负离子模式下，鉴定出63种化合物；正离子模式下，鉴定出54种化合物。所检测到的化合物包括22种鞣质类、28种茋类、6种黄酮类、3种苯丙酸类、2种苯丁酮类和2种有机酸类，其中有53种化合物为在该药材中首次发现，且未发现蒽醌类成分。该方法快速、灵敏，不仅提高了拉萨大黄复杂基质中微量化合物的鉴定效率，同时实现了对拉萨大黄提取物中不同类型化合物的分析鉴别，为进一步阐明拉萨大黄的药效物质基础及质控标准提供了科学依据。

Identification of Chemical Constituents of Rheum Lhasa A. J. Li et P. K. Hsiao by Liquid Chromatography-High Resolution Mass Spectrometry

A method of high performance liquid chromatography tandem high resolution mass spectrometry (HPLC-HRMS) was developed for the separation and identification of chemical components in Rheum lhasaense A. J. Li et P. K. Hsiao extract. The separation of compounds was carried out on an Agilent Zorbax SB-C18 column (150 mm×4.6 mm×5 μm). The mobile phase was composed with acetonitrile and water with the flow rate of 0.5 mL/min. Electrospray ionisation source (ESI) was used, and Rheum lhasaense A. J. Li et P. K. Hsiao extract was analyzed by MS and MSⁿ full scan at positive and negative ion modes. Through comprehensive analysis of the mass spectra and chromatographic behaviors of the compounds, and comparing with the related data from standard substrates, literatures and database, the main chemical components of Rheum lhasaense A. J. Li et P. K. Hsiao extract were deduced and identified. A total of 63 compounds are identified from Rheum lhasaense A. J. Li et P. K. Hsiao extract at negative ion mode, and 54 compounds are identified at positive ionization mode. These compounds contain 22 tannins, 28 stilbenes, 6 flavonoids, 3 phenylpropanoids, 2 butyrophenones and 2 organic acids, which of 53 compounds are firstly discovered in Rheum lhasaense A. J. Li et P. K. Hsiao. And as reported in the literature, enquinones are not found. This method is fast and sensitive, which not only improves the identification efficiency of trace compounds in Rheum lhasaense A. J. Li et P. K. Hsiao complex matrix, but also achieves the analysis and identification of different types of compounds. It is helpful to provide scientific basis for further clarifying the material basis and quality control standards of Rheum lhasaense A. J. Li et P. K. Hsiao.