A simple one-step method for the analysis of monosaccharides including galactosaminitol after acidic hydrolysis is described. The hydrolyzate was re-N-acetylated and analyzed by high-performance anion-exchange chromatography and the sugars were detected by a pulsed amperometric detector. The method was applied on a mixture of neutral oligosaccharides released from mucin glycopeptides of rat small intestine by alkaline borohydride. Sugars were detected down to the nanomole range and the results were compared with monosaccharide compositional analysis performed by gas chromatography of acetylated alditols.