PLGA nanoparticles loaded with doxorubicin hydrochloride (DOX.HCl) were prepared using Biodegradable poly (D, L – lactide-co-glycolide) – 75:25, by o/w and w/o/w emulsification solvent evaporation method using PVA (Mol. Wt. 9000) as surfactant. The encapsulation efficiency of the drug in w/o/w emulsification solvent evaporation method was found to be greatly affected by pH when the experiments were carried out at two pH i.e. 7 and 8. The maximum encapsulation efficiency was found to be 79% . Nanoparticles were morphologically characterized using SEM and particle size analyzer. The average size of the particles was 200nm. Doxorubicin attached PLGA was confirmed by FTIR analysis. In vitro drug release analysis was done at pH 7 and pH 7.4.It was found that drug release was faster at pH 7.