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

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

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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 C18(2。1 mm×100 mm,2。6 μm)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。0 μL;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。
Characterization and identification of chemical constituents in Sedum sarmentosum Bung based on UHPLC-Q-Exactive Orbitrap-MS technology
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 C18 column(2.1 mm×100 mm,2.6 μm)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 3.0 μL.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.

Sedum sarmentosum BungUHPLC-Q-Exactive Orbitrap-MSchemical constituentsflavonoids

朱心仪、杨纯国、田海涛、侯苗、韩利文、邓志鹏

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山东中医药大学药学院,山东济南 250355

山东一方制药有限公司,山东临沂 253000

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

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

山东省中医药科技项目山东省医药卫生科技发展计划项目

M-2023191202213030509

2024

山东科学
山东省科学院

山东科学

CSTPCD
影响因子:0.266
ISSN:1002-4026
年,卷(期):2024.37(5)