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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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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.

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Authors and Affiliations

  1. Department of Chemistry, University of Keele, ST5 5BG, Keele, Staffordshire, UK

    I. D. Wilson & E. D. Morgan

  2. Ecole Normale Superieure, Departement de Biologie, CNRS EP 119, 46 rue d'Ulm, 75230, Paris Cedex O5, France

    R. Lafont

  3. Stine-Haskell Research Center, Dupont Pharmaceuticals, Elkton Road, 19714, Newark, Delaware, USA

    J. P. Shockcor

  4. Biological Chemistry, Biomedical Sciences Division, Imperial College of Science, Technology and Medicine, University of London, South Kensington, SW7 2AZ, London, UK

    J. C. Lindon & J. K. Nicholson

  5. Zeneca Pharmaceuticals, Mereside, Alderley Park, SK10 4TG, Macclesfield, Cheshire, UK

    I. D. Wilson & B. Wright

Authors
  1. I. D. Wilson
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  2. E. D. Morgan
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  3. R. Lafont
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  4. J. P. Shockcor
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  5. J. C. Lindon
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  6. J. K. Nicholson
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  7. B. Wright
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Wilson, I.D., Morgan, E.D., Lafont, R. et al. High performance liquid chromatography coupled to nuclear magnetic resonance spectroscopy and mass spectrometry applied to plant products: Identification of ecdysteroids fromSilene otites . Chromatographia 49, 374–378 (1999). https://doi.org/10.1007/BF02467609

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  • DOI: https://doi.org/10.1007/BF02467609

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