ABSTRACT
Modifications of the standard methods for reduction and acetylation of sugars or methylated sugars (see Volume I) have been directed at decrease in the reaction time and prevention of losses of more volatile components during derivatization. Selvendran et al.5 decreased the time required for acetylation of alditols with acetic anhydride/pyridine to 20 min by heating at 120°C, but there was evidence from response factors that rhamnitol was not completely acetylated under these conditions. Torello et al.,13 in a study aimed at optimizing conditions for analysis of the sugar components of gangliosides by the alditol acetate method, concluded that reduction with NaBH4 in 1 Μ aqueous ammonia (2 mg/ml) for 40 min followed by acetylation with acetic anhydride at 100°C for 30 min, in the presence of the sodium acetate formed on reaction of the excess NaBH4 with acetic acid, gave the best yields of the alditol acetates. After acetylation the samples were dried under a stream of N2 at 38°C to minimize losses of voltile alditol acetates, and this was repeated after removal of the sodium acetate by partitioning between chloroform and water. This procedure permitted analysis of glycolipid sugars in the 1 to 10 μg range.
