We report here the syntheses of galactose-containing polymers via reversible addition-fragmentation chain transfer process. Diblock copolymers with one galactose-containing chain segment and one primary amine-containing or linear glucose-containing chain segment were prepared via chain extension technique. Primary amine pendant groups of the copolymer were further modified with biotinyl-N-hydroxysuccinimide ester. Subsequently, multifunctional glyconanoparticles were prepared and used in the study of biomolecular recognition processes. The biomolecular recognition of the biotin and galactose moiety on the surface of the glyconanoparticles toward avidin and Ricinus communis agglutinin lectin respectively was confirmed using UV-visible spectroscopy and diffractive optics techniques. It was found that both carbohydrate-carbohydrate and carbohydrate-protein interactions increased with increasing divalent salt (Ca2+ and Mn2+) concentration.