摘要
目的:应用超高效液相色谱-四级杆/静电场轨道肼高分辨质谱联用(UHPLC-Q-Orbitrap HRMS)技术,快速识别与鉴定桂枝中水溶性化学成分。方法:采用Waters Acquity UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱。质谱采用ESI源,四级杆/静电场轨道肼质量分析器,正负离子切换扫描采集数据。根据高分辨质谱给出的精确分子量和二级碎片离子等信息,并结合对照品和相关文献对桂枝水提液中的化学成分进行指认。结果:共鉴定桂枝水提液中20个化合物,涵盖苯丙素、苯丙素苷、黄酮、木脂素、倍半萜和小分子酚酸等多种类型的化合物。结论:建立的UHPLC-Q-Orbitrap HRMS方法可快速鉴定桂枝中的化学成分,为深入探讨其药效物质基础、质量控制以及方剂配伍等提供了科学的依据。
Objective:Ultra high performance liquid chromatography coupled with Q-exactive focus hybrid quadrupole and orbitrap high resolution mass spectrometer(UHPLC-Q-Orbitrap HRMS)was applied for identification of water-soluble chemical constituents in Cinnamomum cassia Presl.Method:Chromatographic separation was performed on Waters Acquity UPLC BEH C18 column(2.1 mm×100 mm,1.7μm).The mobile phase consisted of 0.1%formic acid aqueous solution and acetonitrile with a gradient elution.MS and MS/MS spectral analysis were performed on Q-exactive focus hybrid quadrupole and orbitrap mass spectrometer.The mass spectrometer was connected to UHPLC instrument via an HESI interface.Samples were analyzed in positive/negative ionization switching mode.Then the constituents of Cinnamomum cassia Presl were identified by comparing HRMS characteristic data with those of the standard compounds,MS cleavage mechanism and the related literatures.Result:A total of 20 constituents were identified,including phenylpropanoid,phenylpropanoid glycoside,flavonoids,lignans,sesquiterpenes and small phenolic acids.Conclusion:The established UHPLC-Q-Orbitrap HRMS method can be used to identify the chemical constituents of Cinnamomum cassia Presl quickly and accurately,providing the scientific evidence for its quality evaluation and material basis research.
作者
刘瑞
泰刚
王瑞
张淑蓉
Liu Rui;Tai Gang;Wang Rui;Zhang Shurong(Shanxi University of Chinese Medicine,Jinzhong Shanxi 030619;Shanxi Institute For Food and Drug Control,Taiyuan Shanxi 030001)
出处
《山西中医药大学学报》
2021年第1期36-40,共5页
Journal of Shanxi University of Chinese Medicine
基金
山西省科技厅应用基础研究项目(201701D221281)
山西中医药大学科技创新团队项目(2018TD-008)。
