The square-wave voltammetric (SWV) behaviour of riboflavin and folic acid was studied at a static mercury drop electrode by square wave voltammetry. In 0.05 M KCl (pH 5.89) a cathodic scan gave peaks at - 0.56 and - 0.87 V vs. Ag/AgCl for riboflavin and folic acid, respectively. The reduction peak currents are linearly dependent on the concentration of vitamins. Both vitamins can be simultaneously determined from the same voltammogram. The method proposed for the determination of riboflavin and folic acid in multivitamin tablets is very simple, rapid and does not involve time-consuming separation steps. The average contents of riboflavin and folic acid were found to be 14.8 ±1.26% and 1.46 ±2.66%, for tablet A and 9.86 ±1.40% and 1.47 ±2.0% for tablet B, respectively.