基于UPLC-LTQ-Orbitrap-MS^(n)技术的红曲茯苓组方物质基础分析

Chemical constituents in Hongqu Fuling prescription based on UPLC-LTQ-Orbitrap-MS^(n)

目的采用超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用(UPLC-LTQ-Orbitrap-MS^(n))技术对红曲茯苓组方中的化学成分进行定性鉴别,为其确定功效相关质量控制指标提供依据。方法采用Waters ACQUITY UPLC BHEC18(2.1 mm×100 mm,1.7μm),以乙腈-0.1%甲酸水为流动相进行梯度洗脱,柱温35℃,流速0.3 mL·min^(-1),正、负离子模式进行扫描获得高分辨质谱信息。通过与对照品的保留时间及质谱数据信息对比,并结合相关文献报道对相应化合物的相对分子质量、质谱裂解规律进行匹配,对红曲茯苓组方中所含的成分群进行定性分析归类。结果共鉴定了84个化学成分,包括41个黄酮类、11个莫那可林类、10个红曲色素类、8个倍半萜类、4个氨基酸类、2个三萜类、3个多糖类以及5个有机酸类成分,并明确了各化学成分的来源归属以及结合文献报道确定功效相关成分。结论该研究准确地识别了红曲茯苓组方中的化学成分,可为其进一步开发及质量控制提供参考。

Objective To identify the chemical components in Hongqu Fuling prescription and provide a basis for the efficacy related quality control indexes based on ultra-performance liquid chromatography linear ion trap/electrostatic field orbital trap combined high resolution mass spectrometry(UPLC-LTQ-Orbitrap-MS^(n)).Methods The gradient elution was performed on Waters ACQUITY BEH C18 column(2.1 mm×100 mm,1.7μm)with acetonitrile-0.1%formic acid as the mobile phase.The column temperature was 35℃,and the flow rate was 0.3 mL·min^(-1).The scanning was performed in both positive and negative ion modes to obtain high-resolution mass spectrometry information.By comparing the retention time and mass spectrum data with those of the reference substance,and combining with the relevant literature reports,the relative molecular weight and mass spectrum fragmentation law of the corresponding compounds were matched.The component groups in Hongqu Fuling prescription were qualitatively analyzed and verified.Results Totally 84 chemical constituents were identified,including 41 flavonoids,11 monacolins,10 monascus pigments,8 sesquiterpenoids,4 amino acids,2 triterpenoids,3 polysaccharides and 5 organic acids.The source attribution of each component was clear and the efficacy related components were determined based on literature reports. Conclusion The method can identify the chemical components in Hongqu Fuling prescription systematically and accurately, which provide the experimental basis for its further development and quality control .