Glycosaminoglycans (GAGs) are linear, highly negatively charged polysaccharides. They are ubiquitous molecules exhibiting a wide range of biological functions with numerous applications in pharmaceutical, cosmetic, and nutraceutical industrials. The commercial fish-processing industry generates large quantities of solid waste, which can represent a potential resource for GAG production. In this study, we used a three-step recovery and purification scheme for isolation of GAGs from the heads of red salmon (Oncorhynchus nerka). The GAGs recovery yield was 6 to 7 mg from 1 gram of salmon head powder. The recovered GAGs were structurally analyzed with polyacrylamide gel electrophoresis and by disaccharide composition analysis with reversed-phase ion-pair high-performance liquid chromatography. The analyses showed the major composition of the GAGs in red salmon head were chondroitin sulfate C and E.