A simple procedure for combined gas chromatographic analysis of neutral sugars, hexosamines and alditols. Determination of degree of polymerization of oligo- and polysaccharides and chain weights of glycosaminoglycans.

A reliable and reproducible method that allows the combined, simultaneous gas chromatographic (GC) determination of neutral sugars, hexosamines, alditols, identification and quantitation of the reducing aldose end-group in oligo and polysaccharides and glycosaminoglycans has been described. It involves the following steps: release of the reducing end-group from its protein linkage in glycosaminoglycans and reduction of this reducing end-group into alditol, release of the components of the reduced polymer by resin-catalysed hydrolysis, nitrous acid deamination of the resin-bound hexosamines in this hydrolysate into anhydroaldoses and a combined derivatization and GC determination of the neutral sugars as aldononitrile acetates, anhydroaldoses as peracetylated oximes and alditols as alditol acetates. Application of the method to determination of degree of polymerization of oligo-and polysaccharides and chain weights of proteoglycans has been described. This method has several advantages over the previous methods.