摘要
目的:应用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)技术,分析鉴定中药川佛手中的化学成分。方法:采用Thermo Scientific AccucoreTMC18色谱柱(3 mm×100 mm,2.6μm),流动相0.1%甲酸水溶液-0.1%甲酸乙腈溶液梯度洗脱,流速0.3 m L·min-1,柱温30℃。高分辨质谱采用电喷雾离子源(ESI),正离子模式扫描,扫描方式为全扫描/数据依赖二级扫描(Full MS/dd-MS2)。数据运用Compound Discoverer 3.0软件分析,根据化合物的精确相对分子质量、色谱保留时间、特征离子碎片信息,结合mz Cloud网络数据库、中药成分高分辨质谱数据库(OTCML)、文献信息和相关对照品进行鉴定。结果:从川佛手中共鉴定了54个化学成分,包括黄酮类16个,香豆素类17个,柠檬苦素类3个,核苷及其碱基类6个,有机酸类2个,芳香醛类3个,氨基酸类1个,其他类成分6个。结论:该法可全面、准确地分析鉴定川佛手中的主要化学成分,研究结果为阐明川佛手的药效物质基础、优选质量控制指标提供了方法学参考和理论依据,对进一步开发利用川佛手资源具有指导意义。
Objective:To analyze and identify the chemical constituents of Citri Sarcodactylis Fructus by an ultra-high performance liquid chromatography coupled with hybrid quadrupole-orbitrap high-resolution mass spectrometry(UPLC-Q-Orbirap HRMS)method.Method:Compounds were separated on Thermo Scientific Accucore TMC18 column(3 mm×100 mm,2.6μm).The mobile phase was 0.1%formic acid solution and 0.1%formic acetonitrile solution.The flow rate was 0.3 m L·min-1,and the column temperature was set at 30℃.HRMS was performed using an electrospray ion source(ESI),and scanned in a positive ion mode by means of full scan/data dependent secondary scan(Full MS/dd-MS2).Compound Discoverer 3.0 software that could be linked to mz Cloud network database and local high-resolution mass spectrometry database of traditional Chinese medicine components was used to analyze the data,based on accurate molecular mass,retention behaviors and characteristic ion fragmentation of the compounds,as well as literature information and relevant reference materials.Result:Totally 54 chemical constituents in Citri Sarcodactylis Fructus were identified,including 16 flavonoids,17 coumarins,3 limonoids,6 nucleosides and nucleobases,2 organic acids,3 aromatic aldehydes,1 amino acid and 6 other components.Conclusion:The established UPLC-Q-Orbitrap HRMS method can be used to effectively and rapidly identify main chemical constituents of Citri Sarcodactylis Fructus.The findings provide a methodological reference and theoretical foundation for defining the pharmacodynamic material base and optimizing quality control index of Citri Sarcodactylis Fructus,which is of guiding significance for further development and utilization of the resources.
作者
胡瀚文
赵永艳
杨天龙
郑振兴
彭腾
邓放
HU Han-wen;ZHAO Yong-yan;YANG Tian-long;ZHENG Zhen-xing;PENG Teng;DENG Fang(Key Laboratory of Standardization of Chinese Herbal Medicine under Ministry of Education,State Key Laboratory and Breeding Base for Systematic Research Development and Utilization of Chinese Medical Resources,Co-founded by Sichuan Province and Ministy of Science and Technology,School of Pharmacy,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2020年第7期148-155,共8页
Chinese Journal of Experimental Traditional Medical Formulae
基金
四川省科技厅重点研发项目(2018SZ0069).
