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Thiamazole inhibits the thyroid hormone synthesis and does not inactivate the existing thyroxine and triiodothyronine that circulate in the blood. In this paper Thiamazole electrochemical behavior was monitored by cyclic voltammetry on glassy carbon (GC) electrode in the absence and presence of sodium pertechnetate (99mTc). The influence of different Thiamazole concentrations without and in the presence of radiopharmaceutical 99mTc, the effect of the number of scan cycles, and the effect of 99mTc activity on the appearance of cyclic voltammograms were examined. The results show that there is an observed increase in the reduction peak current with an increase of Thiamazole concentration. It was found that the concentration of the tested drug had a significant effect on its redox characteristics. The results obtained show that the application of different concentrations of sodium pertechnetate exhibits the inhibitory properties of the used radiopharmaceutical on the drug in the treatment of thyroid gland disease.