基于UHPLC Q-Exactive Plus Orbitrap HRMS高分辨质谱技术的隔山消提取物化学成分分析

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中文摘要：目的:采用UHPLC Q-Exactive Plus Orbitrap高分辨质谱(HRMS)技术建立全面、快速分析隔山消化学成分的方法,为隔山消的药效物质研究提供科学依据.方法:采用Hypersi 1 GOLD色谱柱(100mm×2.1 mm,1.9 μm),以0.1％甲酸水溶液(A)-0.1％甲酸乙腈溶液(B)为流动相进行梯度洗脱,流速0.3 mL-min-1,柱温40℃.在电喷雾离子源正、负离子模式下采集数据,扫描范围m/z 100～1 500 Da;喷雾电压3.5 kV(+),2.5 kV(-);鞘气流速35 arb;辅助气流速10arb;毛细管温度320 ℃;辅助加热器温度350 ℃.依据HRMS提供的准分子离子峰及碎片离子的精确分子质量信息,结合对照品比对,相关文献报道及m/z Cloud和PUB-chem数据库比对二级质谱进行鉴定.结果:从隔山消提取物中共分析出66个化合物,包括C21甾体类34个,有机酸类13个,苯乙酮类5个,香豆素类4个,生物碱类4个和其他类6个化合物,其中18个化合物为首次在隔山消中报道.结论:该方法可对隔山消化学成分进行快速、准确、全面的定性分析,为今后进一步阐明其药效物质基础和质量控制提供科学依据.

外文标题：Identification of chemical constituents of the extract of Cynanchum auriculatum based on UHPLC Q-Exactive Plus Orbitrap HRMS

外文摘要：Objective:The UHPLC Q-Exactive Plus Orbitrap HRMS technique was used to establish a comprehensive and rapid method for the analysis of the chemical composition of Cynanchum auriculatum and to provide a scientific basis for the study of the medicinal substances of C.auriculatum.Methods:A Hypersi 1 GOLD chromatographic column(100 mm x2.1 mm,1.9 pm)was employed using gradient elution with 0.1％formic acid aqueous solution(A)-0.1％formic acid acetonitrile solution(B)as mobile phase at a flow rate of 0.3 mL·min-1 and a column temperature of 40 ℃.The mass spectrometry was performed using an electrospray ionization and the data were collected in positive and negative ion modes in a scanning range m/z 100～1 500 Da.The spray voltage was set at 3.5 kV(+),2.5 kV(-),sheath gas flow rate was 35 arb,auxiliary gas flow rate was 10 arb,capillary temperature was 320 ℃,and auxiliary heater temperature was 350 ℃.According to the accurate molecular mass information of excimer peaks and fragment ions provided by high-resolution mass spectrometry,combined with reference substance comparison,related literature reports,m/z Cloud,and PUBchem database,comparison of secondary mass spectrometry was conducted to identify the chemical composition.Results:A total of 66 compounds were analyzed from the C.auriculatum extraction,including 34 C21 steroids,13 organic acids,five acetophenones,four coumarins,four alkaloids and six other compounds,among which 18 compounds were reported for the first time in C.auriculatum.Conclusion:The developed method can carry out a rapid,accurate and comprehensive qualitative analysis of the chemical composition of C.auriculatum,and provide a scientific basis for further elucidation of its pharmacodynamic material basis and quality control in the future.

外文关键词：

UHPLC Q-Exactive Plus Orbitrap HRMSCynanchum auriculatumchemical compositionfragmentation rules

作者：

勾健、吴宗芹、孟欣、韦晓毅、刘春花、朱迪、秦兰、孙佳

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作者单位：

贵州医科大学贵州省药物制剂重点实验室/省部共建药用植物功效与利用国家重点实验室,贵阳 550001

贵州医科大学药学院,贵阳 550001

红云制药(贵州)有限公司,凯里 556000

贵州医科大学民族药与中药开发应用教育部工程研究中心,贵阳 550001

贵州中医药大学第一附属医院,贵阳 550001

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关键词：

UHPLC Q-Exactive Plus Orbitrap HRMS 隔山消化学成分裂解规律

基金：

国家自然科学基金项目贵州医科大学博士启动基金项目贵州省科技厅贵阳中医学院第一附属医院联合基金贵阳市科技计划项目

项目编号：

82260811校博合J字[2020]013号黔科合LH字[2017]7147号筑科合同[2019]9-2-33号

出版年：

2024

中国新药杂志

中国医药科技出版社中国医药集团总公司中国药学会

中国新药杂志

CSTPCD北大核心

影响因子：1.039

ISSN：1003-3734

年,卷(期)：2024.33(5)

参考文献量44