In recent years, the presence of numerous xenobiotic substances, such as antibiotics, has been detected in water environments. They can be considered as environmental contaminants, even if their effect on human health has yet to be totally understood. Several approaches have been studied for the removal of these kinds of pollutants. Among these compounds, tetracycline (TC), a broad-spectrum antibiotic, is one of the most commonly found in water due to its widespread use. In the context of reducing the presence of TC in aqueous solution, in this contribution, a composite catalyst based on zinc oxide (ZnO) and iron oxide (γ-Fe₂O₃) was developed and its photocatalytic properties were investigated. The catalytic materials were synthesized by a microwave-assisted aqueous solution method and characterized by Field Emission Scanning Electron Microscope (FESEM), X-Ray Fluorescence (XRF) and Brunauer−Emmett−Teller (BET) analysis. The TC concentration was evaluated by spectrophotometer measurements at specific time intervals. The performed photocatalytic experiments clearly demonstrated that the ZnO/γ-Fe₂O₃ composite catalyst presents significant photocatalytic activity, indeed a TC degradation efficiency of 88.52% was registered after 150 min. The presence of iron oxide in the structure of the catalyst enhances both the surface area and the pore volume, facilitating the adsorption of the analyte on the surface of nanostructures, a fundamental phase to optimize a photodegradation process. Moreover, ZnO was found to play the key role in the photocatalytic process assisted by γ-Fe₂O₃ which enhanced the TC degradation efficiency by 20%.