A general scheme has been developed to determine sugars, starches, and total dietary fiber (TDF) in half-gram freeze-dried subsamples of various foods (or wet samples containing about 0.5 g dry matter). Duplicate subsamples are extracted for free sugars with 80% methanol, dried, derivatized to their trimethylsilylated oximes or ethers, and quantitated by gas-liquid chromatography (GLC). Residues after 80% methanol extraction are incubated with a solution containing amyloglucosidase in acetate buffer. Hydrolyzates are centrifuged, and duplicate aliquots are removed for glucose determination by GLC. Starch content is calculated as glucose (g/100 g) x 0.9. Remaining hydrolyzates are diluted with 4 volumes of 95% ethanol, left at room temperature for 1 h, and then filtered through glass crucibles matted with Celite filter aid. The weight of dry residues are corrected for residual crude protein and ash, and the resulting values are taken to be the TDF content of a sample. A variety of high-consumption foods selected by the Nutrient Data Laboratory of the Agricultural Research Service were analyzed for carbohydrate fractions by this method. Values for total sugar and dietary fiber were compared with those obtained by a commercial laboratory using different methods.