Analysis of Substituted Pyridine-C-Nucleosides by Direct Liquid Introduction Liquid Chromatography/Mass Spectrometry |
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| Authors: | E. L. Esmans M. Belmans I. Vrijens Y. Luyten F. C. Alderweireldt L. L. Wotring |
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| Affiliation: | 1. University of Antwerp (R.U.C.A.), Laboratory for Organic Chemistry , Groenenborgerlaan 171, B-2020, Antwerp, Belgium;2. University of Michigan, College of Pharmacy , Ann Arbor, Michigan, U.S.A. |
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| Abstract: | Abstract A method was elaborated for the analysis of a few original pyridine-C-nucleosides via microbore DLI/LC-MS. The compounds were analyzed on a 10RP8 column (25 cm × 1 mm) using a number of 0.01 M HCOONH4/CH3OH mixtures as eluant. Under appropriate LC-MS conditions, both α- and β-anomers were separated and identified. All nucleosides were characterized by the protonated molecular ion [MH]+, [B+30]+ and [B+44]+-fragment ions. Assignment of the α, β-configuration at C1′ was done with the aid of 13C-NMR. From the DLI/LC-MS data, a semi-preparative HPLC-method was developed to purify the pyridine-C-nucleosides prior to biological evaluation. |
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