A method has been developed for separation and determination of 5 sugars in foods. Mixtures of sugars were separated by high pressure liquid chromatography (HPLC) with a muBondapak/carbohydrate column and acetonitrile-water (80 + 20) as the mobile phase. For the gas-liquid chromatographic (GLC) determination, the sugars were reacted with hydroxylamine hydrochloride to give the oximes, which were then converted to trimethylsilyl derivatives. The derivatives were separated on an 8 ft column containing 3% JXR as the liquid phase. The GLC preparative time was considerably longer than that for HPLC. Both methods were applied to the determination of fructose, glucose, sucrose, maltose, and lactose in processed foods. Recovery studies showed better accuracy for the HPLC method. Because of incomplete derivatization and/or the formation of anomers, the GLC method was not applicable to all foods.