pH-sensitive hydrogels prepared by gamma irradiation find promising biological applications, partially, in the field of localized drug liberation. Herein, optimal conditions for fabricating high-molecular-weight chitosan/polyvinyl alcohol hybrid hydrogels using gamma irradiation at 10, 25, and 30 kGy were investigated by studying the water uptake behavior, the pore size on the surface, and thermal stability. Furthermore, the crosslinking mechanism of irradiated hydrogels was examined via solid-state ¹³C NMR spectrum. The swelling ratio of the gamma-irradiated CS/PVA hydrogel was pH-dependent; particularly, the hybrid hydrogel exhibited high swelling ratios under acidic conditions than those under basic conditions due to the protonation of amino groups on CS-backbone in acidic environments. In addition, amoxicillin was used as a model drug in the in vitro drug release investigations in pH-simulated gastric fluid and deionized water at 37 °C. To identify the drug release mechanism, several kinetic models composing zero-order, first-order, Higuchi, Hixson–Crowell, and Korsmeyer–Peppas models were used. The findings suggested that drug release is mediated by a non-Fickian transport mechanism.

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