Direct 13C NMR Detection in HPLC Hyphenation Mode: Analysis of Ganoderma lucidum Terpenoids
Publikation: Bidrag til tidsskrift › Tidsskriftartikel › Forskning › fagfællebedømt
Solid phase extraction (SPE) was introduced as a crucial step in the HPLC-SPE-NMR technique to enable online analyte enrichment from which proton-detected NMR experiments on submicrogram amounts from complex mixtures were possible. However, the significance of direct-detected (13)C NMR experiments is indubitable in simplifying structural elucidations. In the current study, we demonstrated direct (13)C NMR detection of triterpenoids from a Ganoderma lucidum extract in hyphenation mode. The combined advantage of a cryogenically cooled probe, miniaturization, and multiple trapping enabled the first reported application of HPLC-SPE-NMR analysis using direct-detected (13)C NMR spectra. HPLC column loading, accumulative SPE trappings, and the effect of different elution solvents were evaluated and optimized. A column loading of approximately 600 mug of a prefractionated triterpenoid mixture, six trappings, and an acquisition time of 13 h resulted in spectra with adequate signal-to-noise ratios to detect all C-13 signals.
Originalsprog | Engelsk |
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Tidsskrift | Journal of Natural Products |
Vol/bind | 75 |
Udgave nummer | 5 |
Sider (fra-til) | 876-882 |
Antal sider | 7 |
ISSN | 0163-3864 |
DOI | |
Status | Udgivet - 19 apr. 2012 |
ID: 38131059