<p>In this research, the synthesis and characterization of layered double hydroxides (LDHs) containing different divalent metals (Ni and Co) were studied. Both materials were synthesized by the co-precipitation method and characterized by X-ray diffraction, scanning electron microscopy, and N₂ physisorption. The two hydroxides were evaluated in an advanced oxidation process based on persulfate activation for the degradation of commercial penicillin. The catalysts were tested in their hydroxide form and after calcination as mixed oxides, showing remarkable degradation performance monitored by UV–Vis spectroscopy, with the Ni-based hydroxide achieving at least 70% degradation. The degradation kinetics followed a pseudo-first-order model for the calcined materials and a pseudo-second-order model for the hydroxide form.</p> Graphical abstract <p></p>