摘要：

A methylation-analysis procedure has been developed by which the glycosyl-linkage compositions of microgram quantities of complex carbohydrates, including those containing hexosyluronic acid residues, can be determined. The effectiveness of the procedure was demonstrated by correctly determining the glycosyl-linkage compositions of 1 μg of a disaccharide and 5 μg of an acidic polysaccharide whose structures were unknown to the analyst. The development of a new technique, namely, reversed-phase chromatography on Sep-Pak C18 cartridges, to recover and purify microgram quantities of per-O-methylated complex carbohydrates from methylation-reaction mixtures, was critical to the success of the microscale procedure. The use of gas-liquid chromatography-mass spectrometry with multiple, selected-ion monitoring was also essential for identification and semiquantitation of the partially O-methylated alditol acetates derived from 1 to 5 μg of a complex carbohydrate.

展开