The O-linked N-acetylglucosamine oligosaccharides in the mucins of Trypanosoma cruzi may contain galactofuranose or galactopyranose, depending on the strain, one of the components being the disaccharide. Since galactofuranose is a site for antibody recognition, it is desirable to have a sensitive method for the detection of the galactofuranosyl structures. In this paper, we present procedures for the separation of Galfβ1→ XGlcNAc and Galpβ1→XGlcNAc (X = 3, 4, and 6) as the corresponding alditols by high-pH anion-exchange chromatography with pulse amperometric detection. All the isomeric disaccharides could be resolved on a CarboPac PA-10 column, the galactofuranose-containing disaccharides being more retained in the column. GlcNAcol and Galfβ1→4(Galpβ1→6)GlcNAcol could be analyzed in the same run. The compounds could also be separated by thin-layer chromatography on silica gel 60, a convenient method for analysis of the radiolabeled alditols obtained by reductive β-elimination in the presence of NaB