This paper describes a procedure for the determination of antimony (III) by differential pulse anodic stripping voltammetry using a mercury film screen-printed electrode as the working electrode. The procedure has been optimized using experimental design methodology. Under these conditions, in terms of Residual Standard Deviation (RSD), the repeatability (3.81 %) and the reproducibility (5.07 %) of the constructed electrodes were both analyzed. The detection limit for Sb (III) was calculated at a value of 1.27×10(-8) M. The linear range obtained was between 0.99 × 10(-8) - 8.26 × 10(-8) M. An analysis of possible effects due to the presence of foreign ions in the solution was performed and the procedure was successfully applied to the determination of antimony levels in pharmaceutical preparations and sea water samples.