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[Display omitted] • Heterogenous ferrospinel nanoparticles were prepared towards PMS activation to degrade BTA. • Statistical-based RSM-CCD approach was used for optimization of BTA degradation process. • CoF showed a higher catalytic activity to decompose PMS compared to CuF. • An excellent reusability was observed for the both catalysts after eight consecutive reaction runs. • HO• and SO 4 •– species were responsible for the BTA degradation in both systems. The sulfate radical-based advanced oxidation process has been widely investigated via peroxymonosulfate (PMS) activation in recent years, in which the development of catalysts with high efficiency and stability is crucial. The current work prepared a series of magnetic nanoparticles, including CuFe 2 O 4 (CuF) and CoFe 2 O 4 (CoF), for benzotriazole (BTA) degradation via PMS activation. Various techniques (XRD, VSM, BET, FESEM, and TEM) employed to examine the physicochemical, textural, magnetic, and structural characteristics of the as-prepared catalysts. Moreover, a response surface methodology (RSM) based on central composite design (CCD) used to identify the optimum levels of operational variables and explore the interactions between them. The results showed that 99.7 and 100% of BTA can be removed under optimal conditions when CuF and CoF catalysts were applied in the system in the presence of PMS, respectively. Both catalysts exhibited high degradation efficiencies, even after eight consecutive cycles, highlighting their high stability and reusability in decontamination applications. According to the trapping tests, HO• and SO 4 •– species were responsible for the BTA degradation in both systems. These results suggested that CuF and CoF could be applied as effective recoverable catalysts for activating PMS and degrading persistent pollutants in wastewater treatment. [ABSTRACT FROM AUTHOR]