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Due to a combination of increased urbanization, industrialization, and population growth, many pharmaceutical pollutants are currently being discharged into the environment. A possible strategy is critical for eliminating antibiotic pollutants from the environment, and photocatalysis has been generally recognized as an excellent method for successfully degrading antibiotics at a faster pace. In this work, we employed a hydrothermal synthesis approach to create a novel C3N5/NiCo2S4 Z-scheme-based heterojunction with better interfacial charge transfer and used it as a catalyst for the degradation of norfloxacin antibiotic. The optimized 1:1 C3N5/NiCo2S4 (50CN/NCS) shows the highest photocatalytic efficiency of 86.5% in 120 min towards the degradation of norfloxacin (NOR). Such an effective performance can be attributed to the high responsive nature of photocatalyst in the visible region and superior transfer of interfacial charges via Z-scheme transfer in heterojunction. The high charge transfer efficiency and reduced recombination of charge carriers in heterojunction was confirmed by EIS and PL results. The influence of some key factors such as pollutant concentration, catalyst dosage, pH, and coexisting ions on the photocatalytic activity is also investigated in this work. The optimized heterojunction 50CN/NCS also degraded 89.1%, 78.3%, and 93.2% removal of the other pollutants CIP, SDZ, and BPA, respectively.