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High performance liquid chromatography coupled to nuclear magnetic resonance spectroscopy and mass spectrometry applied to plant products: Identification of ecdysteroids fromSilene otites |
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| Authors: | I. D. Wilson E. D. Morgan R. Lafont J. P. Shockcor J. C. Lindon J. K. Nicholson B. Wright |
| Affiliation: | (1) Department of Chemistry, University of Keele, ST5 5BG Keele, Staffordshire, UK;(2) Ecole Normale Superieure, Departement de Biologie, CNRS EP 119, 46 rue d'Ulm, 75230 Paris Cedex O5, France;(3) Stine-Haskell Research Center, Dupont Pharmaceuticals, Elkton Road, 19714 Newark, Delaware, USA;(4) Biological Chemistry, Biomedical Sciences Division, Imperial College of Science, Technology and Medicine, University of London, South Kensington, SW7 2AZ London, UK;(5) Zeneca Pharmaceuticals, Mereside, Alderley Park, SK10 4TG Macclesfield, Cheshire, UK |
| Abstract: | Summary HPLC coupled in parallel to nuclear magnetic resonance (NMR) and mass spectrometry (MS) has been used to obtain1H NMR and mass spectra of a number of ecdysteroids present in an extract of the plantSilene otites. Reversed phase gradient chromatography was performed using a D20-acetonitrile-based solvent system. NMR and mass spectra were obtained for integristerone A, 20-hydroxyecdysone, 2-deoxy-20-hydroxyecdysone and 2-deoxyecdysone to provide structural confirmation using continuous and stopped flow HPLC-NMR. The combined HPLC-NMR-MS system described here provided a more comprehensive analysis of the ecdysteroids present in the extract than HPLC-NMR alone. |
| Keywords: | Column liquid chromatography NMR spectroscopy and mass spectrometry Plant products Silene otites |
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