Pencycuron is a rather new, non-systemic protective fungicide of the phenylurea class, which is used in the treatment of diseases on various crops and whose residues must therefore, be determined with reliable analytical methods. A rapid, sensitive and reproducible square wave stripping and cyclic voltammetric method applied for the first time for the determination of pencycuron fungicide and it has exhibited a well-defined anodic peak at + 1140 mV (vs Ag/AgCl). A linear relationship has been constructed with a dynamic working range of 0.2-10.0 mg/L on a glassy carbon electrode with a limit of determination and limit of quantification of 0.05 mg/L and 0.17 mg/L, respectively. The simultaneous determination of pencycuron and diethofencarb performed with the relative standard deviations of 4.26% and 1.90% and with the relative errors of 6.00% and + 2.00%, respectively. According to the analytical estimations made in the commercial formulation, pencycuron was obtained as 20.21 +/- 0.32 with a relative standard deviation of 1.58 % and the relative error of + 1.05%, which means that the accuracy and precision is quite good.