基于UHPLC-Q-Exactive Orbitrap-MS技术的垂盆草化学成分表征与鉴定  

Characterization and identification of chemical constituents in Sedum sarmentosum Bung based on UHPLC-Q-Exactive Orbitrap-MS technology

作　　者：朱心仪 杨纯国 田海涛 侯苗 韩利文 邓志鹏 ZHU Xinyi;YANG Chunguo;TIAN Haitao;HOU Miao;HAN Liwen;DENG Zhipeng(College of Pharmacy,Shandong University of Traditional Chinese Medicine,Jinan 250355,China;Shandong Yifang Pharmaceutical Co.,Ltd.,Linyi 253000,China;College of Pharmacy and Pharmaceutical Sciences,Shandong First Medical University(Shandong Academy of Medical Sciences),Jinan 250117,China)

机构地区：[1]山东中医药大学药学院,山东济南250355 [2]山东一方制药有限公司,山东临沂253000 [3]山东第一医科大学(山东省医学科学院)药学与制药科学学院,山东济南250117

出　　处：《山东科学》2024年第5期10-16,共7页Shandong Science

基　　金：山东省中医药科技项目(M-2023191);山东省医药卫生科技发展计划项目(202213030509)。

摘　　要：建立超高效液相-四级杆-静电场轨道阱高分辨质谱法(UHPLC-Q-Exactive Orbitrap-MS),表征与鉴定垂盆草中的化学成分。采用Phenomenex Kinetex C 18(2.1 mm×100 mm,2.6μm)色谱柱,以乙腈-0.1%甲酸水溶液作为流动相进行梯度洗脱,流速为0.3 mL/min,进样量为3.0μL;选择电喷雾离子源,正、负离子模式扫描。根据化合物的保留时间、精确分子量、二级碎片离子、裂解规律及对照品比对进行化合物分析鉴定。结果显示,从垂盆草中共鉴定或初步推导出了53个化学成分,主要包括25种黄酮、12种Megastigmanes类化合物、11种有机酸、3种生物碱及2种其他化合物。其中有5种化合物与对照品比对获得鉴定,3种化合物目前未见报道。该研究建立的UHPLC-Q-Exactive Orbitrap-MS方法可快速且全面表征垂盆草的化学成分,为其质量控制及药效物质基础研究提供参考数据。To develop an ultra-performance liquid chromatograpy-quadrupole electrostatic field orbitrap high-resolution mass spectrometry(UHPLC-Q-Exactive Orbitrap-MS)method for characterization and identification of chemical constituents in Sedum sarmentosum Bung.The separation was performed using a Phenomenex Kinetex C 18 column(2.1 mm×100 mm,2.6μm)with a mobile phase comprising acetonitrile and water containing 0.1%formic acid via gradient elution at a flow rate of 0.3 mL/min;the injection volume was 3.0μL.Mass spectrometry was performed in positive and negative ionization modes with electrospray ionization.The chemical constituents were characterized and identified based on retention time,precise molecular weight,fragment ions,and comparison with the reference substances.The results of this study showed that 53 compounds were characterized and identified in Sedum sarmentosum Bung,including 25 flavonoids,12 megastigmanes,11 organic acids,3 alkaloids and 2 other compounds.Five of these compounds were identified via comparison with reference compounds,and three compounds may have not been reported from Sedum sarmentosum Bung.The UHPLC-Q-Exactive Orbitrap-MS method proposed in this study can rapidly and comprehensively characterize the chemical constituents in Sedum sarmentosum Bung and provide a reference basis for the research on quality control and atherapeutic material basis of Sedum sarmentosum Bung.

关 键 词：垂盆草 超高效液相-四级杆-静电场轨道阱高分辨质谱法 化学成分 黄酮 

分 类 号：R284[医药卫生—中药学]