The voltammetric behaviors of 1-(3-Fluoro-benzenesulfonyl)-5-{3-[5-(3-methoxy-phenyl)-2-methyl-2H-[1,2,4]triazol-3-yl]-phenyl}-1H-indole (5b) have been investigated in Britton- Robinson (B-R) buffer pH 7.0 using differential pulse voltammetry (DPV), anodic stripping voltammetry (ASV) and cyclic voltammetry (CV) on a glassy carbon electrode νs Ag/AgCl reference electrode. The preliminary observation for 5b was investigated using DPV technique in B-R buffer pH 7, a broad differential pulse voltammetric oxidation wave at E_a= 0.65V was observed. The voltammetric oxidation process has been shown to be irreversible and the diffusion is controlled with adsorption characteristics. The developed anodic stripping voltammetric (ASV) was used to study some optimized experimental conditions such as accumulation time, accumulation potential, scan rate, frequency, pulse amplitude, other working electrodes and convection rate. A calibration curve for 5b was studied from 2×10^-6 to 3×10^-5M (correlation coefficient = 0.994, n=8) under optimum conditions and the detection limit was 8×10^-8M. The used anodic stripping voltammetric method shows a good reproducibility (n=8) for 5b with relative standard deviation RSD% was 0.54% and a good stability. An accuracy of the developed ASV was evaluated via the mean recovery of 97%±1.0. Some interference, usually present in pharmaceutical compounds, has been also evaluated. The analytical applications of the developed ASV technique were carried out for a direct determination of 5b in medical preparations and biological fluids.