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A high-efficiency strategy integrating offline two-dimensional separation and data post-processing with
Wenlong Wei1, Jinjun Hou1, Changliang Yao1
1Shanghai Research Center for Modernization of Traditional Chinese Medicine, National Engineering Laboratory for TCM Standardization Technology, Shanghai Institute of Materia Medica, Chinese Academy of Science, Shanghai 201203, China.
Journal of Chromatography. A
|July 1, 2019
Summary
A new two-dimensional liquid chromatography/ultra-high performance supercritical fluid chromatography tandem mass spectrometry method efficiently identifies bufadienolides in traditional Chinese medicine. This approach aids in discovering new natural compounds and analyzing isomers.
Area of Science:
- Natural Product Chemistry
- Analytical Chemistry
- Pharmacognosy
Background:
- Accurate chemical analysis of traditional Chinese medicine (TCM) is crucial for efficacy and safety.
- Discovering novel natural compounds from TCM is vital for drug development.
- Interpreting complex data from two-dimensional liquid chromatography (2D LC) can be challenging.
Purpose of the Study:
- To establish an efficient off-line 2D LC/UHPSFC-Q-TOF/MS system for bufadienolide analysis.
- To apply Global Natural Product Social Molecular Networking (GNPS) for rapid dereplication.
- To characterize bufadienolides and discover new compounds in Venenum Bufonis.
Main Methods:
- Developed an integrated 2D LC/UHPSFC-Q-TOF/MS method.
- Fractionated Venenum Bufonis extract using reversed-phase HPLC.
- Analyzed fractions using UHPSFC-Q-TOF/MS and processed data with GNPS.
Main Results:
- Characterized 229 bufadienolides, including two novel subclasses, in Venenum Bufonis.
- Identified two new compounds, confirmed by NMR.
- UHPSFC demonstrated excellent isomer separation capabilities.
Conclusions:
- The combined 2D LC/UHPSFC-Q-TOF/MS and GNPS strategy significantly improves efficiency in detecting new compounds.
- This integrated approach enhances the observation of isomers from natural sources.
- The method validates the feasibility for comprehensive analysis of complex natural products.
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