Feedstuffs high in water-soluble materials such as sugars, corn-syrup solids, molasses, urea, lactic acid, or glycerol are weighed, extracted first with water, and dried prior to exhaustive extraction with Soxhlet or continuous (Goldfisch) extraction utilizing dry ethyl ether as solvent. Solvent is evaporated, and residue is dried to constant weight at 100°. Weight is corrected by reagent blank and expressed as % crude fat or ether extract. This method is applicable to mixed feeds that have not been heat-treated, baked, or expanded. It is not applicable to dried milk products or feeds containing high levels of urea.