CoBi2O4 (CBO) nanoparticles were synthesized by sol-gel method using Polyvinylpyrrolidone (PVP) as a complexing reagent. For a single-phase with the spinel structure, the formed gel was dried and calcined at four temperatures stages. Various methods were used to identified and characterized the obtained spinel, such as X-ray diffraction (XRD), Scanning Electron Micrograph (SEM-EDX), Transmission electron microscope (TEM), Fourier transform infrared (FT-IR), X-ray fluorescence (XRF), Raman and UV-Vis spectroscopies. The photocatalytic activity of CBO was examined for the degradation of a pharmaceutical product Cefixime (CFX). Furthermore, for the prediction of the CFX degradation rate an artificial neural network model was used.The network was trained using the experimental data obtained at different pH with different CBO doses and initial CFX concentrations. To optimize the network, various algorithms and transfer functions for the hidden layer were tested. By calculating the REVISED MANUSCRIPT mean square error (MSE), 13 neurons were found to be the optimal number of neurons and produced the highest coefficient of correlation R 2 of 99.6 %. The relative significance of the input variables was calculated and the most impacting input was proved to be the initial CFX concentration. The effects of some scavenging agents were also studied. The results confirmed the dominant role of hydroxyl radical OH • in the degradation process. With the novel CoBi2O4/ZnO hetero-system, the photocatalytic performance has been enhanced, giving an 80% degradation yield of CFX (10 mg/L) at neutral pH in only 3 hours.