BACKGROUND: Metronidazole (MNZ) is a highly typical representative antibiotic widely occurring in wastewaters. Its release poses potential threats to the environment and human health. Advanced oxidation processes based on heterogeneous catalysis are promising technologies for organic matter removal. In this study, a new type of magnetic mesoporous FeCo 2 O 4-Fe 3 O 4 microrods was prepared and evaluated as catalyst to activate peroxymonosulfate (PMS) for metronidazole (MNZ) degradation. RESULTS: The effects of catalyst dosage, PMS concentration, and pH on MNZ degradation were investigated. A 96.8% removal of MNZ (100 mg L −1) was attained in the FeCo 2 O 4-Fe 3 O 4 /PMS under the optimum conditions of 4 mM PMS, 0.4 g L −1 FeCo 2 O 4-Fe 3 O 4 loading, pH 7 and 60 min reaction time. The hydroxyl radicals (•OH) and sulfate radicals (SO 4 •−) were identified as the primary reactive species attributed to MNZ removal. The plausible mechanism of the catalytic degradation was proposed and assumed to be related to the Co/Fe species that exerted the synergistic effect during reactions. FeCo 2 O 4-Fe 3 O 4 showed excellent reusability and stability, which was testified by the successive degradation experiments. More importantly, FeCo 2 O 4-Fe 3 O 4 exhibited general applicability in eliminating various antibiotics, including ciprofloxacin, 2,4-dichlorophenol, ofloxacin, and tetracycline. The efficiencies of which were 78.8%, 77.1%, 81.3%, and 60.7%, respectively, under identical reaction conditions as MNZ. CONCLUSION: This study proved that mesoporous FeCo 2 O 4-Fe 3 O 4 microrods are efficient PMS activators and provided a novel strategy for developing FeCo 2 O 4-based catalysts for the removal of organic pollutants from water.