To investigate the radio impurity in the radiolysis of 18F-FDG at high radiodose and radioconcentrated solutions and develop methods of repurification. The radiolysis of 18F-FDG was analyzed by TLC. The radio-impurity was confirmed by biodistribution and small animal PET/CT studies. 18F-FDG was unstable at high radioconcentrition over 37 GBq/mL or under basic condition. TLC, biodistribution and PET/CT all
indicated that the main autoradiolysis byproduct was free fluoride ion. The radiolyzed 18F-FDG was repurified by solid-phase extraction (SPE) column. The repurified 18F-FDG had a radiochemical purity (RCP) of over 99% and significantly lower bone uptake than that was before repurification
(P = 0.0003). There was a positive correlation between the recovery yield and the purity of 18F-FDG (R2 = 0.66).