This chapter presents the Gas-Liquid Chromatographic Analysis of Constituent Carbohydrates in Glycoproteins. Application of gas-liquid chromatography (GLC) to the analysis of steroids, fatty acids, Krebs cycle and allied acids, amino acids, and carbohydrates is presented. The conditions of cleavage, derivatization, and GLC provide a quantitative determination of the commonly found glycoprotein sugars, that is, L-arabinose, L-fucose, D-xylose, D-mannose, D-galactose, D-glucose, N-aeetyl-D-galactosamine, N-acetyl-D-glucosamine, and the neuraminic acids as the N-acetyl derivatives. The chapter describes a general procedure, allowing quantitation of the above-mentioned sugar components, along with two modifications. One modification involves cleavage under mild conditions to determine the neuraminic acid and fucose values. The second modification, under more vigorous conditions, involves assessing total recovery of the amino sugars. For some glycoproteins the general procedure determines all the expected components quantitatively, but this cannot be assumed to be the case with all samples until verified by the modifications. The GLC carried out on a dual-column instrument with a flame-ionization detector and the 0-trimethylsilyl (TMS) ether sugar derivatives.