Characterization by gas-liquid chromatography-mass spectrometry and proton-magnetic-resonance spectroscopy of pertrimethylsilyl methyl glycosides obtained in the methanolysis of glycoproteins and glycopeptides

Abstract

The quantitative analysis by gas chromatography of monosaccharides present in glycoproteins and glycopeptides using methanolysis, followed by re-N-acetylation and trimethylsilylation, gives rise to several peaks for each monosaccharide. The identity of these peaks for xylose, fucose, mannose, galactose, glucose, N-acetylglucosamine, N-acetylgalactosamine and N-acetylneuraminic acid was established for alpha- and beta-methyl pyranosides and furanosides by combined g.l.c.-mass spectrometry and proton-magnetic-resonance spectroscopy. These data provide for the unambiguous interpretation of the gas chromatograms obtained in the application of this g.l.c. method, and supply basic information for the further application of mass spectrometry in this field.

1H-N.m.r. study of enzymically generated wheat-endosperm arabinoxylan oligosaccharides: structures of hepta- to tetradeca-saccharides containing two or three branched xylose residues

“…spectrum of 41 ( Fig. 3) pointed to the presence of a single diarabinosylxylopentaose, AX-41, with the Xylp residues p (J1, [2][3][4][5][6][7][8] and the Arafresidues a (J,,2 -1 Hz)'~. On the various H-l tracks of the constituent monosaccharides in the 2D HOHAHA spectrum (Fig.…”

Molecular characterization of the Aspergillus nidulans treA gene encoding an acid trehalase required for growth on trehalose

“…In these conditions trehalose, glucose, mannitol and glycerol eluted at 6.7, 8.0, 9.0 and 12.0 min, respectively. The nature of the soluble sugars in the peak fractions was confirmed after trimethylsilylation by gas liquid chromatography using a DELSI 200 apparatus with a capillary column (25 m × 0.2 mm internal diameter; Villeneuve Saint Georges) filled with dimethyl siloxane (DB-1); gas vector: helium, pressure 0.7 bar; column temperature 100-260ЊC at 2ЊC min ¹1 (Kamerling et al, 1975). When radioactive samples were analysed, the HPLC ionexclusion column was coupled to a flow scintillation analyser (Radiomatic Flow-one/␤; Packard) using Ultima Flow AP scintillation fluid (Packard) at a 1.5 ml min ¹1 flow rate.…”

Isolation and partial characterization of rat gastric mucous glycoprotein

“…Quantitative analysis of the sugars by gas-liquid chromatography was performed as described by Kamerlingh et al [20]. Samples were hydrolyzed in methanolic 1 M HC1 for 24 h at 85°C.…”