In order to investigate the formation of organic salts of drugs, two new salts of pindolol were precipitated using benzoic acid and 2-methoxyphenylacetic acid. The reversed-phase high-performance liquid chromatographic (HPLC) method was developed for the determination of the mole ratio of the salt components. The method permits the simultaneous quantitation of the cationic and anionic parts of the salts prepared. The method was validated with respect to linearity and precision of the chromatographic run and the assay. Also, the precisions at the lowest and the highest levels of the linearity curves were tested. The system suitability was studied by calculating the chromatographic parameters, such as capacity factor (k′), number of theoretical plates (N), tailing factor (T) and resolution (R) between pindolol and organic acids used.