This report describes the development and application of a flow photocatalytic reactor for the effective photodecomposition of organic compounds and the recovery of a targeted metal ion; specifically, we describe the decomposition of a gallium-ethylenediaminetetraacetic acid (Ga-EDTA) complex. The system includes a scrubber, which increases the amount of dissolved oxygen in the solution before entering the photocatalytic reactor. First, the decomposition efficiency of the developed reactor is evaluated using dimethyl sulfoxide (DMSO). The decomposition of DMSO is accelerated upon introducing oxygen from the scrubber into the flowline. Second, we employ this system for the decomposition of Ga-EDTA and evaluate the recovery of a Ga radioisotope (RI), which can serve as a probe in positron emission tomography for medical diagnoses. The byproducts generated during Ga-EDTA photodecomposition are monitored by capillary electrophoresis, and the released Ga3+ concentrations are determined by inductively coupled plasma atomic emission spectroscopy for the stable isotope of Ga and with a scintillation detector for RI-Ga. After 30 min under ultraviolet irradiation, 54 % of the RI-Ga released during the photodecomposition of RI-Ga-EDTA was recovered.