The biochemical and medical importance of glycoproteins necessitates a development of efficient separations and high-sensitivity measurements for glycans and glycopeptides, which are formed as the result of controlled enzymatic degradation of glycoproteins in complex mixtures.Monitoring changes in glycan profiles and microheterogeneities at the sites of glycosylation becomes important in glycoprotein structural studies and a search for disease biomarkers.In aiding a complete structural elucidation, glycopeptide separations must be op timized, so that both hydrophilic and hydrophobic entities are recovered for mass-spectrometric (MS) analysis.While the utility of graphitized carbon media was recently demonstrated for glycan analyses, here we extend their uses for glycopeptide separations and compare them with the results obtained with the reversed-phase LC chips.