Metabisulfite is used as an antioxidant agent in a number of pharmaceutical formulations. In order to quantify simultaneously both metabisulfite and its oxidation product (sulfate), a capillary zone electrophoretic (CZE) method with indirect UV detection was developed. Best results were achieved with a background electrolyte (BGE) constituted of 15 mM pyromellitic acid, 15 mM tris-(hydroxymethyl)-aminomethane and 0.2 mM tetradecyltrimethylammonium bromide at pH 8.3 and an applied electrical field of 123 V/cm in a 32.5 cm fused silica capillary. Indirect UV detection was performed at a wavelength of 225 nm. In order to validate this method, an internal standard (IS), namely ammonium formate, was used. Moreover, due to the high chloride concentration in the pharmaceutical formulation, conductivity was adjusted by adding sodium chloride into standard solutions to prevent matrix effect. Linearity and accuracy were successfully tested in a concentration range of 33.3-250 microg/ml for sodium metabisulfite and of 50-375 microg/ml for sodium sulfate. Method precision was determined on six samples each day. Thereby, relative standard deviations (R.S.D.) of 6% and 12-13% were obtained for intra-day and inter-day precision, respectively. Considering the instability of metabisulfite and its use as an antioxidant agent and not as an active principle, the method was accepted and used for routine analyses.