Poly (vinyl alcohol)/poly(acryl amide-co-acrylamidoglycolic acid) (PVA/Poly(Am-co-AGA) based pH sensitive semi interpenetrating (semi-IPN) hydrogels were prepared by free radical polymerization in aqueous solution using N, N-methelene-bis-acryl amide (MBA) as a crosslinker. Different hydrogels with different compositions of AGA and MBA were prepared and characterized by Fourier transform infrared spectroscopy. The developed hydrogels were used for controlled release of 5-fluorouracil (5-FU). The drug entrapment efficiency up to 55% was achieved. The 5-FU loaded gels were characterized by X- ray diffraction and differential scanning calorimetric techniques, to understand the nature of drug in the polymeric matrix. The release of 5-FU through the semi-IPN was completed with in similar to 12 h. Swelling studies performed in water have been analyzed with the help of an empirical equation to investigate the diffusion mechanism.