The objective of this work was to develop and validate a fast and reproducible method which is able to determine the concentration of ketoconazole in raw materials and tablets. The samples were analyzed by dynamic thermogravimetry at heating rates of 10, 20, 40, 60 and 80°C min−1 in nitrogen and nitrogen-synthetic air mixture. The concentrations of ketoconazole in the raw material and in the tablets were obtained from the vapor pressure curves. The data showed that there is no significant difference between the vapor pressure profiles of ketoconazole itself and in its tablet in both studied environmental conditions confirming that the process is really vaporization. The concentration of ketoconazole was determined in the raw material and tablets of the drug.