H/D isotopic exchange in the fast atom bombardment of ecdysteroids

Píš, Jaroslav; Vaisar, Tomáš

doi:10.1002/(sici)1096-9888(199711)32:10<1050::aid-jms557>3.0.co;2-0

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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

et al. 1999

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SummaryHPLC coupled in parallel to nuclear magnetic resonance (NMR) and mass spectrometry (MS) has been used to obtain 1H NMR and mass spectra of a number of ecdysteroids present in an extract of the plant Silene 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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