UHPLC-Q-Exactive Orbitrap MS结合离子排除列表快速鉴定侗药马卡列丙中化学成分

doi:10.16333/j.1001-6880.2020.2.009

天然产物研究与开发 ›› 2020, Vol. 32 ›› Issue (2): 250-256.doi: 10.16333/j.1001-6880.2020.2.009

UHPLC-Q-Exactive Orbitrap MS结合离子排除列表快速鉴定侗药马卡列丙中化学成分

李凯琳1，熊佩1，龚开妍1，彭婕1，史思林1，蔡伟1,2,3*

1湖南医药学院药学院；2新型抗体药物及其智能运输系统湖南省重点实验室；3侗医药研究湖南省重点实验室，怀化 418000

出版日期:2020-02-29 发布日期:2020-04-23
基金资助:
国家自然科学基金青年项目（81603393）；湖南省自然科学基金青年项目（2018JJ3376）；湖南省教育厅资助科研项目（19A353）

Rapid characterization of constituents in Duhaldea nervosa based on UHPLC-Q-Exactive Orbitrap MS combined with exclusion list technique

LI Kai-lin1,XIONG Pei1,GONG Kai-yan1,PENG Jie1,SHI Si-lin1,CAI Wei1,2,3*

1School of Pharmaceutical Sciences,Hunan University of Medicine;2Hunan Province Key Laboratory for Antibody-based Drug and Intelligent Delivery System,Hunan University of Medicine;3Hunan Provincial Key Laboratory of Dong Medicine,Hunan University of Medicine,Huaihua 418000,China

Online:2020-02-29 Published:2020-04-23

摘要/Abstract

摘要： 为进一步阐明侗药马卡列丙中未知的化学成分，采用UHPLC-Q-Exactive Orbitrap MS快速分析侗药马卡列丙中的化学成分。色谱柱为Thermo Scientific Hypersil GOLD（100 mm×2.1 mm，1.9 μm），流动相为0.1%甲酸水-乙腈，梯度洗脱，流速为0.3 mL/min，进样量为2 μL，负离子模式下，采用一级母离子全扫描和数据依赖性前三强二级子离子扫描并结合排除离子列表模式（Full Scan MS/dd-MS2/Exclusion list）采集数据。通过对照品，参考文献和数据库从侗药马卡列丙中共鉴定出40个化合物，均为从该植物中首次发现。该方法可以快速、有效、准确地对侗药马卡列丙中化学成分进行分析，为侗药马卡列丙的质量控制和药效物质基础研究奠定基础。

关键词: 马卡列丙, UHPLC-Q-Exactive Orbitrap MS, 成分鉴定, 离子排除列表

Abstract: To investigate the unknown constituents of Duhaldea nervosa by UHPLC-Q-Exactive Orbitrap MS combined with exclusion list technique.The analysis was performed on a Thermo Scientific Hypersil GOLD (100 mm×2.1 mm,1.9 μm),with a mobile phase consisting of 0.1% formic acid in water and acetonitrile for gradient elution.The flow rate was 0.3 mL/min and the injection volume was 2 μL.The data was acquired in negative mode at full scan and at the MS2 data triggered by data-dependent MS2 combined with exclusion list scanning.Finally,a total of 40 constituents was identified by comparing the reference compounds,bibliography data and database.To our best knowledge,it is the first time to report those compounds from Duhaldea nervosa.A rapid,effective,and accuracy method was built to study the constituents of Duhaldea nervosa in this study,which will be very helpful for the further study in quality control and material basis.

Key words: Duhaldea nervosa, UHPLC-Q-Exactive Orbitrap MS, identification, exclusion list

中图分类号:

R284.1

李凯琳1，熊佩1，龚开妍1，彭婕1，史思林1，蔡伟1,2,3*. UHPLC-Q-Exactive Orbitrap MS结合离子排除列表快速鉴定侗药马卡列丙中化学成分[J]. 天然产物研究与开发, 2020, 32(2): 250-256.

LI Kai-lin1,XIONG Pei1,GONG Kai-yan1,PENG Jie1,SHI Si-lin1,CAI Wei1,2,3*. Rapid characterization of constituents in Duhaldea nervosa based on UHPLC-Q-Exactive Orbitrap MS combined with exclusion list technique[J]. NATURAL PRODUCT RESEARCH AND DEVELOPMENT, 2020, 32(2): 250-256.

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UHPLC-Q-Exactive Orbitrap MS结合离子排除列表快速鉴定侗药马卡列丙中化学成分

Rapid characterization of constituents in Duhaldea nervosa based on UHPLC-Q-Exactive Orbitrap MS combined with exclusion list technique

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