Gas chromatographic determination of monosaccharides such as L-arabinose, L-rhamnose, D-xylose, D-mannose, D-galactose, and D-glucose was studied. The recovery of sugars under hydrolysis condition was examined by GLC (Fig. 1) and was found to be almost quantitative when steroidal glycosides were hydrolyzed with N sulfuric acid in dioxane-water (1 : 3) solution (Table III). A simple and accurate method by GLC was thus presented for the individual determination of sugar components in the micro amounts (5-10 mg) of steroidal saponins. The molar ratios of sugar components were determined on the new convallasaponins by this method (Table V).