Guaiacol is an undesired compound in some natural products, mainly because of its aroma.In this work, the voltammetric determination of guaiacol by oxidation at a carbon paste electrode following a cathodic accumulation was first tried, with no sucess, because there was no accumulation of the compound. On the contrary, it was found that there is accumulation of a product formed after oxidation of guaiacol, probably a dimeric product, that can be determined by reduction. Using an accumulation time of 5 minutes and a potential at which guaiacol is being oxidized, a determination limit of 2 u.g/L was obtained by cathodic stripping voltammetry, a value about ten times lower than that obtained in the anodic determination. The method was applied to the determination of guaiacol in cork stoppers.