DETERMINATION OF STRUCTURE OF DISACCHARIDES AS O-TRIMETHYLSILYL DERIVATIVES OF DISACCHARIDE ALDITOLS BY GAS-LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY

A method is described for the structural analysis of disaccharides by gas-liquid chromatography (g.l.c.)-mass spectrometry. A disaccharide mixture is reduced to the corresponding alditols, and analyzed as the O-trimethylsilyl derivatives by g.l.c. Simultaneous recording of the mass spectra allows the determination of the position of the intermolecular bond, the molecular weight, and certain other structural details. The use of borodeuteride instead of borohydride in the reduction stage is essential for the interpretation of the mass spectra. The monosaccharide components are identified by g.l.c. after isolation of the O-trimethylsilyl derivatives of the disaccharide alditols by small-scale, preparative g.l.c. The method is applied to the analysis of disaccharides containing both simple and amino sugars. © 1969.