From Retrospective Assessment to Prospective Decisions in Natural Product Isolation: HPLC-SPE-NMR Analysis of Carthamus oxyacantha

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• 作者：Kenneth T. Johansen ; Sileshi G. Wubshet ; Nils T. Nyberg ; Jerzy W. Jaroszewski
• 刊名：Journal of Natural Products
• 出版年：2011
• 出版时间：November 28, 2011
• 年：2011
• 卷：74
• 期：11
• 页码：2454-2461
• 全文大小：310K
• 年卷期：v.74,no.11(November 28, 2011)
• ISSN：1520-6025

文摘

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 ¹H and ¹³C chemical shifts.