Thermal formation of free radicals in flumetasone sterilized according to the pharmaceutical norms at 160, 170 and 180 °C was examined by electron paramagnetic resonance (EPR) spectroscopy. The microbiological analysis was done. Similar free radical concentrations were measured for flumetasone sterilized at 160 and 170 °C. The concentration was considerably higher than that for flumetasone sterilized at 180 °C. Fast spin-lattice relaxation processes, homogeneously broadened EPR lines, and complex free radicals system characterize the heated flumetasone. Free radicals were not observed 30 days after thermal sterilization. Optimal temperatures of sterilization of flumetasone are 160 and 170 °C.