The polymerization film of Congo red was prepared on the surface of carbon paste electrode by electropolymerization using cyclic voltammetric method. The higher catalytic activity was obtained for electrocatalytic oxidation of Dopamine, with drastic enhancement of the reversibility and peak current in 0.2 phosphate buffer solution of pH 7.0 at the sweep rate 100 mV/s. The variation of sweep rate and pH were investigated. The limit of detection of Dopamine was found to be 0.06 μM. The effect of interference studies was done by differential pulse voltammetric technique. In the simultaneous look at, Dopamine and Uric acid were well separated by cyclic voltammetric technique. The proposed method showed good sensitivity, selectivity, and reproducibility.