Cellulose powder / poly (N-vinyl-2-pyrrolidone) (CP/PVP) and carboxymethylcellulose / poly (N-vinyl-2-pyrrolidone) (CMC/PVP) hydrogels were synthesized at different reaction conditions using ammonium persulphate as initiator. The optimum reaction conditions to prepare such gels are PVP molecular weight (40000 Dalton), PVP concentration (60%), APS/polymers weight ratio (100%), reaction time (45 min), reaction temperature (90 OC), as well as CP/PVP or CMC/PVP weight ratio (25%). The prepared matrices were characterized via FTIR as well as scan electron microscope analysis. The release profiles of sodium diclofenac form the CP/PVP and CMC/PVP gels at pH 7 were studied. Release studies showed burst release for both matrices at first 30 min followed by sustained behavior. matrices PVP/CMC showed highest release of DS due to repulsive forces between polymer chains.