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A comparative study of Cu-impregnated ZnO and Ni-impregnated ZnO for the sonophotocatalytic degradation of cefixime in aqueous solution under visible light irradiation was carried out. Sonophotocatalysts were prepared by using a wet impregnation method and characterised using different spectroscopic techniques. Sonophotocatalytic efficiency of degradation is superior to photolysis, sonolysis, photocatalysis and sonocatalysis. Different operational parameters like pH, catalyst dosage, different enhancers, scavenger's effect, initial concentration of drug, reusability of catalyst and catalyst settling time were optimised. Optimum time of 30 min was found for the 45.7% degradation of cefixime using Cu-ZnO and 42.2% degradation using Ni-ZnO photocatalysts at pH 10. The degradation of cefixime increased from 75.3% to 100% with 5 mmol of hydrogen peroxide using 0.1 g/ L of Cu-ZnO and 99.8% using 0.15 g/L of Ni-ZnO, while other oxidising agents were found less effective using (Cu–ZnO-Ni-ZnO) photocatalyst. A very little decrease in degradation was observed with different types of scavengers. Catalyst reusability was checked up to three cycles and good results up to three cycles were achieved and followed pseudo-first-order kinetic model. Furthermore, the sonophotocatalytic activity was tested for real pharmaceutical wastewater resulting in 91 and 89% removal of total organic carbon (TOC) using (Cu-ZnO-Ni-ZnO), respectively. The proposed method was successfully applied on commercial and synthetic sample with satisfactory results. [ABSTRACT FROM AUTHOR]