In this work, efficient adsorbents for β-lactam antibiotics based on mesoporous iron oxide containing surface [FeO x (OH) y ] sites were produced by controlled precipitation of iron hydroxide and thermal treatment at 150, 200, 300 and 450 °C (150FeOH, 200FeOH, 300FeOH and 450FeOH, respectively). Mössbauer, X-ray diffraction (XRD), thermogravimetry-mass spectrometry (TG-MS), Fourier transform infrared spectroscopy (FTIR), Raman, Brunauer-Emmett-Teller method (BET), scanning electron microscopy (SEM) and elemental analyses showed that the temperature caused a gradual dehydroxylation process with a significant increase of the mesoporous surface area (e.g., 114-142 m 2 g-1 with 46-59% mesopores, i.e., 0.04-0.09 cm 3 g-1) and approximate compositions of FeO 1.06 (OH) 0.89 for 150FeOH up to FeO 1.38 (OH) 0.26 for 450FeOH. The material 150FeOH showed high adsorption capacities of ca. 42 and 58 mg g-1 for amoxicillin and ceftriaxone, respectively. Experiments assessing the effect of NO 3-, Cl-, competitive PO 4 3adsorption and H 2 O 2 decomposition suggest that the [FeO x (OH) y ] surface sites located in the mesopores are involved in the efficient adsorption by complexation of the β-lactam antibiotics.