Three new methods are reported for the gas chromatographic analysis of di- and trisaccharides. Method I: Sugars are converted into their methoximes by reaction with methoxylamine hydrochloride in pyridine, followed by esterification with acetic anhydride. The separation is performed on OV 225 at 260 degrees C. Method II: Disaccharides are reduced to the alditols with sodium borohydride in aqueous solution, followed by acetylation with acetic anhydride in pyridine. In this method, only one peak is observed for each sugar. The derivatives are separated on OV 225 at 260 degrees C. Method III: Sugars are converted into their methoximes by reaction with methoxylamine hydrochloride in pyridine, followed by trifluoroacetylation with N-methyl-bis (trifluoroacetamide). The trisaccharide derivatives still show sufficient volatility. The separation is performed on OV 101 at 130 degrees C for disaccharides, and at 160 degrees C for trisaccharides. The retention times for biologically occurring di- and trisaccharides such as maltose, maltotriose, lactose, and sucrose are reported. The reliability criteria for method I are reported for the analysis of lactose, maltose and sucrose.