For the first time, Fe-zeolite 5A (Fe-Z5A) efficacy in the UV-assisted ozonation process to remove ciprofloxacin (CF) in wastewater is investigated. FTIR, SEM, EDX, BET, and the mass transfer process for point of zero charge are used to characterize the catalyst. Furthermore, the synergic process (UV/O3/Fe-Z5A) is compared with O3, O3/UV, and Fe-Z5A/O3 processes. The influence of catalyst dose, hydroxyl radical scavenger, and off-gas ozone released is discussed. The removal efficiency of CF in wastewater (for the synergic process) is compared with a single ozonation process. The results indicate that the synergic process was more efficient than others, with about 73% CF being removed (in 60 minutes) in the synergic process. The results also show that synergic processes produce less off-gas ozone than other processes, suggesting more ozone consumption in the synergic process, and confirmed by the radical scavenger effect and hydrogen peroxide decomposition studies. The Fe-Z5A was found to operate through a hydroxyl mechanism in which Fe worked as an active site that promotes the formation of hydroxyl radicals. Finally, the synergic process was more efficient than the ozonation process in the wastewater matrix. Hence, Fe-Z5A/O3/UV pathway is highly efficient for the degradation of pharmaceuticals in wastewater.