Abstract: Sugars and sugar alcohols are widely distributed natural compounds with high boiling and melting points. Chemical and instrumental analysis of sugars and sugar alcohols needs to derivate them into their derivatives. In this study, 1-methylimidazole was used as solvent and catalyst, hydroxylamine hydrochloride and acetic anhydride were used as reagent for oximization and acetylation, respectively. The optimal temperature and time for the reaction of derivation were determined through the experiments. The effect of the components and the proper dosage of sugar and sugar alcohol were discussed. The products of the derivation reaction were separated effectively by gas chromatography with a capillary column, detected by a FID detector and structurally identified and characterized by GC-MS. The result of GC-FID and GC-MS shows that sugars and sugar alcohols can be acetylated completely under optimized conditions. The result of GC-FID analysis shows that sugars and sugar alcohols can be separated, detected and quantitatively determined.