The analysis of two-dimensional proton shift-correlated 500 MHz NMR spectra of several peracetylated glycosphingolipids confirmed that peracetylated oligosaccharides are particularly well suited for the identification of the constituent sugar residues and the elucidation of the sites of glycosidic linkage. Although a number of partial sequences could be determined by inter-residue nuclear Overhauser effect or long-range scalar coupling across the glycosidic bonds, the full sequence determination of larger oligosaccharides has several limitations owing to experimental dilficulties and possible ambiguities in assignments due to signal overlap. The following peracetylated glycosphmgolipids were investigated by two-dimensional methods at