Spectrophotometric, atomic absorption spectrometric and high performance liquid chromatographic (HPLC) procedures have been developed for the determination of betahistine hydrochloride and captopril. The three procedures are based on the reaction of the drugs with carbon disulphide in alkaline medium with the formation of the dithiocarbamate or the trithiocarbonate derivative of betahistine (BHT) and captopril (CAP), respectively, then subsequent chelation with divalent metals. The absorbance measurement of the formed chelates or of the metal moiety of chelates was used as the basis for the spectrophotometric and atomic absorption spectrometric determinations. The formed complexes have been used as pre-column derivatizing procedure for the HPLC determination of the two drugs. The different experimental conditions were optimized. The calibration graphs were linear over the applicable concentration ranges. The proposed procedures were applied successfully for the determination of the two investigated drugs in their tablets dosage form.