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Electron impact and chemical ionization (CH,, iso-C,H,, and NH,) mass spectra of some tetra-acetylated anomeric glycosides have been examined with a view to the characterization of anomeric pairs. Minor differences observed in the relative intensities of common ions in the anomeric pairs in the electron impact mass spectra are found to be enhanced in the methane and isobutane chemical ionization mass spectra. In the absence of thermal decomposition, the p-anomers show greater ion abundances of common glycosyl ions than the a-anomers. Ammonia chemical ionization mass spectra show complementary behaviour indicating strong adduct ions and practically no fragmentation.

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