An ultra high performance liquid chromatography coupled with hybrid quadrupole-orbitrap mass spectrometry （UHPLC-quadrupole-orbitrap MS） method was developed to systematically analyze chemical constituents of Scutel...An ultra high performance liquid chromatography coupled with hybrid quadrupole-orbitrap mass spectrometry （UHPLC-quadrupole-orbitrap MS） method was developed to systematically analyze chemical constituents of Scutellaria barbata D. Don. The 70% methanol extract was separated on an Agilent Eclipse Plus Cl8 column （1.8μm, 150 mm×2.1 mm）, and eluted with a gradient of methanol-acetonitrile-water containing 0.1% formic acid at a flow rate of 0.25 mL/min. Constituents were identified by HRMS in the negative ion mode using both full scan and two-stage threshold-triggered mass modes. A total of 56 compounds, including 20 free flavonoids, 20 flavonoid O-glycosides, 2 flavonoid C-glycosides, 4 phenylethanoid glycosides, and 10 phenolic compounds were identified by analyzing their high resolution mass spectral data. Among them, 8 flavonoids and 2 phenylethanoid glycosides were unambiguously identified by comparing with reference standards. This study demonstrates that hybrid quadrupole-orbitrap mass spectrometry is a powerful tool in structural identification of unknown compounds in comolicated herbal extracts.展开更多
Objective:The objective of this study was to establish a systematic method for rapidly classifying and recognizing the chemical constituents of Biejiajian pill(BJJP)for safety in clinical applications.Materials and Me...Objective:The objective of this study was to establish a systematic method for rapidly classifying and recognizing the chemical constituents of Biejiajian pill(BJJP)for safety in clinical applications.Materials and Methods:Ultra-high-performance liquid chromatography coupled with hybrid quadrupole-Orbitrap mass spectrometry(MS)was used for chemical profiling and identification of BJJP components.The chromatographic effluents were detected by MS in positive and negative ion modes.Results:A total of 217 compounds were structurally identified by deducing the mass fragmentation patterns and comparing with reference compounds and data reported in the literature,including 84 flavonoids,49 phenolic constituents,30 terpenoids,24 triterpenoids,7 alkaloids,6 anthraquinones,and 17 other compounds.Conclusions:The established method can rapidly identify and analyze the chemical components of BJJP,laying the foundation for further analysis of active compounds,quality control,and metabolite fingerprinting.展开更多
基金National Natural Science Foundation of China(Grant No.81222054 and 21305005)the Program for New Century Excellent Talents in University from Chinese Ministry of Education(Grant No.NCET-11--0019)National Science and Technology Mega Project for Primary Drug Innovation of China(Grant No.2014ZX09304--307)
文摘An ultra high performance liquid chromatography coupled with hybrid quadrupole-orbitrap mass spectrometry （UHPLC-quadrupole-orbitrap MS） method was developed to systematically analyze chemical constituents of Scutellaria barbata D. Don. The 70% methanol extract was separated on an Agilent Eclipse Plus Cl8 column （1.8μm, 150 mm×2.1 mm）, and eluted with a gradient of methanol-acetonitrile-water containing 0.1% formic acid at a flow rate of 0.25 mL/min. Constituents were identified by HRMS in the negative ion mode using both full scan and two-stage threshold-triggered mass modes. A total of 56 compounds, including 20 free flavonoids, 20 flavonoid O-glycosides, 2 flavonoid C-glycosides, 4 phenylethanoid glycosides, and 10 phenolic compounds were identified by analyzing their high resolution mass spectral data. Among them, 8 flavonoids and 2 phenylethanoid glycosides were unambiguously identified by comparing with reference standards. This study demonstrates that hybrid quadrupole-orbitrap mass spectrometry is a powerful tool in structural identification of unknown compounds in comolicated herbal extracts.
基金supported by the National Natural Science Foundation of China(No.82474493)China Postdoctoral Science Foundation(No.2022M711085)+2 种基金Natural Science Foundation of Henan Province(No.232300420053No.222300420222)the Special Project of the National Clinical Research Base of TCM(No.2022JDZX096)。
文摘Objective:The objective of this study was to establish a systematic method for rapidly classifying and recognizing the chemical constituents of Biejiajian pill(BJJP)for safety in clinical applications.Materials and Methods:Ultra-high-performance liquid chromatography coupled with hybrid quadrupole-Orbitrap mass spectrometry(MS)was used for chemical profiling and identification of BJJP components.The chromatographic effluents were detected by MS in positive and negative ion modes.Results:A total of 217 compounds were structurally identified by deducing the mass fragmentation patterns and comparing with reference compounds and data reported in the literature,including 84 flavonoids,49 phenolic constituents,30 terpenoids,24 triterpenoids,7 alkaloids,6 anthraquinones,and 17 other compounds.Conclusions:The established method can rapidly identify and analyze the chemical components of BJJP,laying the foundation for further analysis of active compounds,quality control,and metabolite fingerprinting.
