Combined gas-liquid chromatography-mass spectrometry (GC-MS) has been used for the analysis of 2-amino-2-deoxy-d-glucose, 2-amino-2-deoxy-d-galactose, their methyl glycosides, and the corresponding alditols, as well as of the N-acetylated forms. The compounds were analyzed as trimethylsilyl (TMS) derivatives synthesized by using chlorotrimethylsilane and hexamethyldisilazane in pyridine, or using these reagents together with bis(trimethylsilyl)acetamide. In the latter procedure, the free amino groups, in addition to the hydroxyl groups, are also trimethylsilylated. Identification of the derivatives was based on their retention times in gas-liquid chromatography and their mass-spectral characteristics. The value of GC-MS of TMS derivatives in the analysis of polysaccharides is discussed. © 1969.