In this study we performed the dynamic and static scintigraphy of the domestic dog, using the newly synthesized radiopharmaceutical, [99mTc(CO)3(H2O)3]-C60(OH)22-24. In the current study, an advanced one-step method for the functionalization of fullerenol by 99mTc is described. Optical properties of as-prepared samples and the mechanism responsible for the functionalization were investigated using UV–VIS and FTIR spectroscopy, respectively. Also, the presence of the Tc complex on fullerenol was confirmed by using the energy dispersive X-ray spectroscopy, HPLC and MALDI TOF techniques.This simple and effective method of producing a new radiopharmaceutical is of interest not only for its application in various areas of technology and biology, but also for investigating its potential use in radiation technology for nanoengineering of materials. With dynamic scintigraphy, performed during 30 minutes (120 frames, 15 sec per frame), we obtained ratios of heart, liver and spleen counts: 222/249/168; 178/320/217; 120/348/239 respectively. By static scintigraphy after 1 hour, we detected the activity in heart, liver, spleen and intestines. After 4 hours, the radiopharmaceutical activity was detected in salivary glands. The detection after 21 hours showed the activity in kidneys and urinary bladder, while the activity in intestines was absent. After 24 hours, we detected the activity in liver, spleen, kidneys and urinary bladder. Pharmacokinetic investigations performed in this study are of key interest for the further fullerenol in vivo research.