In this study, the glycosylation of human transferrin (as a model of PSA) and PSA are investigated by HPAE-PAD using <10 μg of protein. Two methods are utilized to evaluate protein glycosylation. One method is used to investigate the N-linked oligosaccharides and glycan sialylation. A second method evaluates the potential presence of O-linked glycans by monitoring monosaccharide composition. By using a combination of acid hydrolysis and enzymatic digestion steps prior to HPAE-PAD analysis, information about the glycosylation, as well as linkages within the glycans, is determined.