基于2种色谱-质谱联用技术的参芪降糖颗粒化学成分分析

目的基于UPLC-Q/TOF MS和GC-MS法分析参芪降糖颗粒的化学成分。方法参芪降糖颗粒甲醇提取液采用Zorbax RRHD SB C₁₈(100 mm32.1 mm,1.7μm)色谱柱,以乙腈-水为流动相进行梯度洗脱,体积流量0.3 mL/min。电喷雾离子源正负离子模式下对色谱流出物进行质谱检测,利用Peakview软件,根据二级质谱信息及文献,对主要色谱峰进行鉴定分析。参芪降糖颗粒挥发性成分分析采用HP-5MS毛细管柱(60 m3250μm30.25μm),程序升温,EI离子源,质量扫描范围m/z 25~500。GC-MS分析通过NIST 2014标准谱库检索并结合文献对参芪降糖颗粒中挥发性成分进行快速鉴定。结果参芪降糖颗粒中共鉴定出132个非挥发性成分和86个挥发性成分。结论提供了一种快速、有效、全面系统地对参芪降糖颗粒的化学成分进行定性分析的方法,为参芪降糖颗粒药效物质基础研究、二次开发、质量控制、药理作用机制研究等奠定基础。

Analysis of chemical constituents of Shenqi Jiangtang Granule based on UPLC-Q/TOF MS and GC-MS

Objective To study the chemical constituents of Shenqi Jiangtang Granule(参芪降糖颗粒) based on UPLC-Q/TOF MS and GC-MS. Methods The methanol extract of Shenqi Jiangtang Granule was separated on Zorbax RRHD SB C₁₈ column(100 mm× 2.1 mm, 1.7 μm), and the gradient elution of acetonitrile-water was used as mobile phase at a flow rate of 0.3 m L/min. The chromatographic effluent was detected by mass spectrometry under the positive and negative ion modes of the ESI source. According to the cleavage fragments of MS/MS and literaturea, the main chromatographic peaks were identified by Peakview software. Composition analysis of volatile oil from Shenqi Jiangtang Granule was performed by HP-5MS column(60 m × 250 μm × 0.25 μm), with programmed temperature and EI ion source, and the mass scanning range was m/z 25—500. GC-MS analysis was performed using the enhanced NIST 2014 standard spectrum library for rapid identification of volatile components in Shenqi Jiangtang Granule. Results A total of 132 non-volatile components and 86 volatile components were identified in Shenqi Jiangtang Granule. Conclusion This study provides a rapid and effective method for the qualitative analysis of the chemical components of Shenqi Jiangtang Granule comprehensively and systematically, which lays the foundation for the research on the material basis of pharmacodynamics, secondary development, quality control, and pharmacological mechanism.