By adapting previously reported reaction conditions, [18F]FMISO was synthesized using a TracerLab FX‐FDG module in 31 min from no carrier added [18F]fluoride in 56% radiochemical yield. A novel and simple purification setup based on disposable cartridges was developed allowing the radiopharmaceutical to be obtained in high radiochemical purity (>99.5%) and with chemical impurities far below the Ph.Eur.'s thresholds. Moreover, the study pinpointed some shortcomings of the high‐performance liquid chromatography (HPLC) method reported in the dedicated Ph.Eur's monograph.
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