Air-calcined electrospun CuO nanoparticles embedded in TiO2 nanofibers were synthesized and examined for tetracycline photodegradation. The electrospun nanofibers were characterized by XRD, FESEM, ICP, EDX, N2 adsorption–desorption, PL, and UV–DRS techniques. Elemental analysis, crystalline phase identification method, and FESEM images proved electrospun 0D/1D composite nanofiber fabrication. Composite nanofibers have mesoporous structure, extended light response range, limited band gap energy, promoted light absorption, and efficient charge transfer. Excess CuO produces a surface covering of TiO2 nanofibers, which decreases textural characteristics and increases agglomerations. CuO inclusion caused a hump-like variation in tetracycline UV photodegradation, culminating at 10 wt.%. RSM-CCD optimized process parameters for photocatalytic performance. A quadratic model (Adj. R2 = 0.9986, p-value < 0.0001) predicted experimental data and interpreted system behaviour. TiO2-CuO (10%) nanofibers eliminated 86% and 77% of tetracycline under UV and simulated sun light, respectively, under optimum conditions (photocatalyst dose of 1.4 g.L-1, initial solution pH of 6.14, and 75 min irradiation).
