In this paper a rapid method of anodic stripping voltammetry (ASV) coupled with experimental design was developed for simultaneous determination of Zn2+, Cd2+, Pb2+, and Cu2+ in gasoline samples. A microwave assisted gasoline digestion procedure for sample preparation was also established. The determination limit was found to be 0.24 mu g L-1 for Zn2+; 8.58 x 10(-4) mu g L-1 for Cd2+; 0.13 mu g L-1 for Pb2+, and 0.87 mu g L-1 for Cu2+. It was found that the interferences of concomitant metal ions were negligible. Gasoline samples collected in the city of Sao Luis (MA), Brazil were analyzed using this developed method, and the results demonstrated that this method was reliable and accurate. It is expected that this method can be used as a routine technique for metal ion determination in gasoline. (C) 2011 Elsevier Ltd. All rights reserved.