超高效液相色谱-四极杆-飞行时间质谱分析匙羹藤化学成分

Analysis of chemical constituents in Gymnema sylvestre(Retz.)Schult via ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry

目的:基于超高效液相色谱-四极杆-飞行时间质谱(ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry,UPLC-Q-TOF-MS/MS)技术分析匙羹藤的化学成分。方法:采用Waters CORTECS UPLC T_(3)色谱柱(150 mm×2.1 mm,1.6μm)以0.1%甲酸-乙腈的流动相梯度洗脱,电喷雾负离子模式下对色谱流出物进行检测,检测范围m/z 50~2000。结果:通过高分辨质谱数据(一级质谱及二级质谱碎片)分析,结合数据库、文献以及对照品比对,共鉴别出101种成分,包括53种三萜类、37种黄酮类、5种有机酸类、3种单萜类、1种二萜类、1种菲类、1种甾体类化合物。结论:本研究通过UPLC-Q-TOF-MS/MS技术快速鉴别了匙羹藤的化学成分,该方法快速、准确、简便,能够用于匙羹藤化学成分的定性鉴定,为该草药的质量标准以及物质基础研究奠定基础。

Objective:Ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS/MS)was used to analyze the chemical constituents of Gymnema sylvestre(Retz.)Schult.Methods:A Waters CORTECS UPLC T_(3)(150 mm×2.1 mm,1.6μm)column was utilized to separate the components using the mobile phase at a gradient elution of 0.1%formic acid-acetonitrile and the effluent was detected in electrospray anionic mode with the detection range of m/z 50~2000.Results:Combined with the databases,literature,and reference standards,we identified 101 components,including 53 triterpenoids,37 flavonoids,5 organic acids,3 monoterpenoids,1 diterpenoid,1 phenanthrene,and 1 steroid based on the analysis of high-resolution mass spectrometry data(primary mass spectra and secondary mass spectral fragments).Conclusion:The chemical constituents of Gymnema sylvestre were identified using the fast,accurate,and simple UPLC-Q-TOF-MS/MS method for qualitative identification,which laid the foundation for establishing a quality standard of the herb and its material basis research.