Rapid characterization of polysaccharides from marine animals using chemical degradation combined with liquid chromatography mass spectrometry.

Glycosaminoglycans of marine origin have exceptional biological activities, but rapid elucidation strategies for precise structures are still lacking. In this study, the optimal conditions for deacetylation of glycosaminoglycans were optimized first. The hydrazinolysis time of 24 h was determined as the final condition, oligosaccharides with a degree of polymerization of 2-14 are mainly produced after hydrazinolysis. Then mixed oligosaccharides generated by deacetylation-deamination cleavage of polysaccharides were detected with hydrophilic interaction chromatography with tandem mass spectrometry (HILIC-MS/MS), and the total ion chromatography showed excellent resolution. The mass spectrometry data were automatically processed by GlycReSoft, and the corresponding matching results were obtained according to the set parameters. A small amount of keratan sulfate exists in oligosaccharides of Teuthida and Salmo salar, and ion peaks corresponding to IdoA-GalNAc4S exist in oligosaccharides of Scophthalmus maximus and Salmo salar. The results of the manual analysis of the mass spectrometry data verified that the HILIC-MS/MS combined with automatic analysis by software adopted in this study could achieve accurate matching and matching of mixed oligosaccharide components. The establishment of a rapid and accurate analysis strategy for the structure of glycosaminoglycans in this study will help the development of its application and standardized industrial production.