A simple, rapid, selective and sensitive electrochemical method for the direct determination of prednisolone in spiked human serum and tablets was developed. The electrochemical oxidation and determination of prednisolone has been carried out at glasy carbon electrode (GCE) in various aquaeous solution in the pH range of 0.56-12.30 by cyclic (CV) and Osteryoung square wave voltammetry (OSWV). The best results were obtained for the determination of prednisolone by OSWV method in 0.5 mol L-1 sulphuric acid at about pH 0.56. The peak current and peak potential depends on pH, so its influence and also scan rate were studied. The diffusion controlled by nature of the peak was established. This electroanalytical procedure enabled to determine prednisolone in the concentration range 1.0 X 10(-6)- 2.0 x 10(-5) mol L-1. This limit of detection (LOD) and limit of quantification (LOQ) were obtained as 3.4x10(-7) and 4.5x 10(-7) mol L-1 respectively. Precision and accuracy of the developed method were checked by recovery studies in spiked tablets and human serum.