基于超高效液相色谱-四级杆-静电场轨道阱质谱的胃复春片化学成分研究
2020-08-07周丹丹邹秦文林瑞超
周丹丹 邹秦文 林瑞超



摘要 目的:基于超高效液相色谱-四级杆-静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)技术对胃复春片的物质基础进行了全面的研究,对主要化学成分进行快速鉴定。方法:采用Thermo Hypersil GOLD C18色谱柱(4.6 mm×150 mm,3 μm),以0.05%甲酸水-乙腈为流动相的梯度洗脱进行分离。质谱采用正、负离子检测模式、全扫描及自动触发二级质谱扫描功能(Full MS/dd MS2)采集数据。通过化合物的最大紫外吸收波长、精确相对分子质量及二级碎片离子信息,与对照品的保留时间、mzVault 2.0质谱数据库及相关文献报道进行比对,鉴定胃复春片的主要化学成分。结果:共鉴定出164种化学成分,其中包括人参皂苷类42个、黄酮类97个、二萜类19个、其他6个。结论:UPLC-Q-Orbitrap HRMS技术能够快速、准确、较全面地鉴定胃复春片中化学成分,为明确药效物质基础研究及提升质量标准提供了理论依据。
关键词 胃复春片;化学成分;UPLC-Q-Orbitrap HRMS;人参皂苷;黄酮;二萜
Abstract Objective:Based on ultra-high performance liquid chromatography-quadrupole-orbitrap mass spectrometry(UPLC-Q-Orbitrap HRMS)technology,to thoroughly study the material basis of Weifuchun Tablets,and to quickly identify the main chemical components.Methods:The analysis was performed on a Thermo Hypersil GOLD C18 column(150 mm×4.6 mm,3 μm).The mobile phase comprised of water containing 0.05% formic acid and acetonitrile was used for gradient elution.Mass spectrometry adopts positive and negative ion detection mode,full scan and automatic trigger secondary mass spectrometry scan function(Full MS/dd MS2)to collect data.By comparing the compound′s maximum ultraviolet absorption wavelength,accurate relative molecular mass and secondary fragment ion information with the reference substance retention time,mzVault 2.0 mass spectrometry database and related literature reports,the main chemical components of Weifuchun tablets were identified.Results:A total of 164 chemical constituents including 42 ginsenosides,97 flavonoids,19 diterpenoids and 6 other compounds,were identified.Conclusion:UPLC-Q-Orbitrap HRMS technology can quickly,accurately,and comprehensively identify the chemical composition of Weifuchun tablets,which provides a theoretical basis for clarifying the basic research of drug efficacy and improving quality standards.
Keywords Weifuchun Tablet; Chemical Constituents; UPLC-Q-Orbitrap HRMS; Ginsenosides; Flavonoids; Diterpenoids
中圖分类号:R284.1文献标识码:Adoi:10.3969/j.issn.1673-7202.2020.13.001
胃复春片收载于《中华人民共和国药典》[1]2015年版一部,由红参、香茶菜、麸炒枳壳3味中药组成,临床上主要用于慢性萎缩性胃炎、胃癌前期病变、浅表性胃炎、胃十二指肠溃疡的治疗[2]。中药复方的化学成分研究有助于明确中药药效物质基础,是提升质量标准的基础,具有十分重要的意义。目前,胃复春片中化学成分研究的报道较少。钟静华[3]采用HPLC-DAD-ESI-MSn以及HPLC/Q-TOF-MS技术对胃复春片进行分析,共鉴定出60个化学成分,初步明确了其化学物质基础。超高效液相色谱串联高分辨质谱技术具有多种质谱扫描方式,其高灵敏度、高分辨率及高质量准确度等特点,能够实现对复杂的中药复方中化学成分的筛查、识别和快速鉴定[4-5]。……
