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Microscale methodology for structure elucidation of natural products
1Department of Chemistry and Biochemistry and Skaggs School of Pharmacy and Pharmaceutical Sciences, University of California, San Diego, 9500 Gilman Drive MC0358, CA 92093, USA. tmolinski@ucsd.edu
Microscale spectroscopic techniques like microcryoprobe NMR and circular dichroism (CD) enable the discovery of new molecules at nanomole and picomole levels. These complementary methods aid in natural product structure elucidation from extreme environments.
Area of Science:
- Natural Product Chemistry
- Analytical Chemistry
- Spectroscopy
Background:
- Microscale spectroscopic techniques have advanced significantly.
- Microcryoprobe Nuclear Magnetic Resonance (NMR) allows for the discovery and structure elucidation of new molecules at nanomole quantities.
- Newer methods in Circular Dichroism (CD) have extended detection limits to picomole levels.
Purpose of the Study:
- To highlight the complementary nature of NMR and CD for stereostructure elucidation.
- To showcase the synergistic potential of integrated microprobe NMR, microscale degradation, and synthesis.
- To emphasize the expanded scope for discovering bioactive natural products from extreme sources.
Main Methods:
- Microcryoprobe NMR spectroscopy for molecular discovery and structure elucidation.
- Circular Dichroism (CD) spectroscopy for high-sensitivity detection.
- Microscale degradation and synthesis techniques integrated with spectroscopy.
Main Results:
- NMR and CD are complementary tools for complete stereostructure elucidation of complex natural products.
- These integrated microscale methods enable discovery of compounds from challenging sources.
- Detection limits have been pushed to nanomole (NMR) and picomole (CD) levels.
Conclusions:
- Integrated microprobe NMR, microscale degradation, and synthesis are powerful synergistic tools.
- These techniques open new avenues for discovering bioactive natural products from uncultured microbes, rare invertebrates, and environmental samples.
- Advances in microscale spectroscopy significantly enhance natural product discovery capabilities.
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