From retrospective assessment to prospective decisions in natural product isolation: HPLC-SPE-NMR analysis of Carthamus oxyacantha
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From retrospective assessment to prospective decisions in natural product isolation : HPLC-SPE-NMR analysis of Carthamus oxyacantha. / Johansen, Kenneth T; Wubshet, Sileshi G; Nyberg, Nils T; Jaroszewski, Jerzy W.
I: Journal of Natural Products, Bind 74, Nr. 11, 28.11.2011, s. 2454-2461.Publikation: Bidrag til tidsskrift › Tidsskriftartikel › Forskning › fagfællebedømt
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TY - JOUR
T1 - From retrospective assessment to prospective decisions in natural product isolation
T2 - HPLC-SPE-NMR analysis of Carthamus oxyacantha
AU - Johansen, Kenneth T
AU - Wubshet, Sileshi G
AU - Nyberg, Nils T
AU - Jaroszewski, Jerzy W
PY - 2011/11/28
Y1 - 2011/11/28
N2 - 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 (1)H and (13)C chemical shifts.
AB - 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 (1)H and (13)C chemical shifts.
KW - Former Faculty of Pharmaceutical Sciences
U2 - 10.1021/np200780m
DO - 10.1021/np200780m
M3 - Journal article
C2 - 22060189
VL - 74
SP - 2454
EP - 2461
JO - Journal of Natural Products
JF - Journal of Natural Products
SN - 0163-3864
IS - 11
ER -
ID: 35457116