Gas chromatography was used after trimethylsilyl derivatization to determine the composition of soapstocks from corn germ and peanut oil refining. Soap fatty acids, polyalcohols, small carbohydrates, sterols, steryl glycosides, mono-, di- and triglycerides were measured using a hexamethyldisilazane/pyridine preparation and a high-temperature capillary column. Additional peaks associated with the fatty acids appeared in the chromatograms when pyridine was incorporated into the sample preparation. Limiting the concentration of soapstock in the sample or replacing pyridine with a chlorinated solvent reduced the formation of these artifacts.