Analysis Of Substituted Pyridine-C-Nucleosides By Direct Liquid Introduction Liquid-Chromatography Mass-Spectrometry

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.