A simple method based on capillary zone electrophoresis was proposed for the analysis of ephedrine and pseudoephedrine in various commercial food supplements. The proposed method is suitable for a rapid identification and determination of ephedrine and pseudoephedrine in complex matrix of analyzed samples. The described extraction into 5 mM aqueous HCl proved right for a complete release of ephedrine and pseudoephedrine from the analyzed substance. An acidic carrier electrolyte (pH 3.6) containing b-alanine, aspartic acid and heptakis(2,6-di-O-methyl)-ß-cyclodextrin) is the method of choice for complete resolution of both alkaloids.