NMR ANALYSIS OF OLIGOSACCHARIDES

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The samples were analyzed for monosaccharide composition by preparing the trimethylsilyl derivatives of the methylglycosides followed by gas chromatography (GC) and combined gas chromatography/mass spectrometry (GC-MS) analysis. TMS methylglycosides were prepared from the sample by methanolysis in 3 M HCl, re-N-acetylation of amino sugars with pyridine and acetic anhydride in methanol, and per-O-trimethylsilylation with Tri-Sil. GC analysis of the TMS methylglycosides was performed on an HP5890 GC using a DB1 fused silica capillary column. GC-MS analysis was performed using an HP5890 GC interfaced to a 5970 MSD. Monosaccharides were identified by their retention times in comparison to standards, and the carbohydrate character of these was authenticated by their mass spectra.