Journal
JOURNAL OF NATURAL PRODUCTS
Volume 74, Issue 11, Pages 2454-2461Publisher
AMER CHEMICAL SOC
DOI: 10.1021/np200780m
Keywords
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Funding
- Drug Research Academy
- Faculty of Pharmaceutical Sciences
- University of Copenhagen
- Bruker BioSpin
- Danish Agency for Science, Technology and Innovation
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An extract of Carthamus oxyacantha (wild safflower) was investigated using two approaches: a traditional, nontarget fractionation by VLC and HPLC, and the hyphenated technique HPLC-PDA-HRMS-SPE-NMR followed by targeted isolation of selected constituents for inclusion in a screening library of pure natural products. While the nontarget fractionation involved considerable time spent on pursuing fractions containing well-known or undesired compounds, the hyphenated analysis was considerably faster and required less solvent and other consumables. The results were used to design and execute an optimized, HPLC-HRMS-guided, targeted isolation scheme aiming exclusively at a series of identified spiro compounds. Thus, HPLC-PDA-HRMS-SPE-NMR is a dereplication technique of choice, allowing economical acquisition of comprehensive data about compounds in crude extracts, which can be used for rational, prospective decisions about further isolation efforts. A total of 15 compounds were identified in the extract. Six Spiro compounds, of which four have not previously been characterized, and tracheloside (a lignin glucoside) are presented with assigned H-1 and C-13 chemical shifts.
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