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Cu2O@CuxFeyO4 nanohybrids (NHs) have been electrosynthesized by a simple and environmentally safe method to be used as catalysts for tetracycline degradation. NHs shown an average diameter of 14(5) nm and exhibit high crystallinity with spherical morphology. XPS results demonstrate a cuprite-enriched surface; meanwhile, the inner layer is composed by a nonstoichiometric copper spinel structure. The degradation has been monitored by UV–Visible spectroscopy, TOC analysis, and HPLC. The electrochemical characterization demonstrates the synergetic effect of Fe3+/Fe2+ and Cu2+/Cu+ coupling to enhance the activation of persulfate. This effect results in a greater degradation efficiency of NHs than other catalysts, namely, CuxOy, Fe3O4, and a mixture of both and Cu2O. It has been found that a previous adsorption stage before degradation does not improve the elimination of the pollutant and its length in time, with a TOC reduction of 72.6 % in 2 h. Conversely, conducting the oxidative process in a direct step resulted in a more rapid and efficient process, 82.3 % of reduction in 1 h. Through this method, the catalyst reutilization resulting in a decrease of 50 % in TOC degradation from the third use, while the TCY concentration degraded remains almost constant. This reduced catalytic activity with use might be a consequence of 1) the absence of the single Cu-oxide layer due to the leaching of mainly Cu ions but also Fe ions during the degradation tests, and, 2) the passivation of the outermost layer, mainly covered by C–O species and OH groups, which hinders access to active catalyst sites. © 2023 The Author(s)