This research aims to assess the presence of four antibiotic compounds detected in the influent and effluent of wastewater treatment plants (WWTPs) in the POCTEFA territory (north of Spain and south of France) during the period of 2018–2019, and to relate the removal of antibiotic compounds with the processes used in the WWTPs. The performance of a photocatalytic TiO₂/UV-VIS pilot-scale plant was then evaluated for the degradation of selected antibiotics previously detected in urban treated effluent. The main results reflect that azithromycin had the highest mass loadings (11.3 g/day per 1000 inhabitants) in the influent of one of the selected WWTPs. The results also show considerable differences in the extent of antibiotics removal in WWTPs ranging from 100% for sulfadiazine to practically 0% for trimethoprim. Finally, the photocatalytic TiO₂/UV-VIS pilot-scale plant achieved the removal of the four antibiotics after 240 min of treatment from 78%–80% for trimethoprim and enrofloxacin, up to 100% for amoxicillin, sulfadiazine and azithromycin. The catalyst recovery via mechanical coagulation–flocculation–decantation was almost total. The Ti concentration in the effluent of the TiO₂/UV-VIS pilot-scale plant was lower than 0.1% (w/w), and its release into the environment was subsequently minimized.

Water monitoring is key to determining the presence of potentially hazardous substances related to urban activities and intensive farming. This research aimed to perform a long-term (four years) quantitative monitoring of selected antibiotics (azithromycin, enrofloxacin, trimethoprim and sulfadiazine) both in rivers and wastewaters belonging to the Ebro River basin (North of Spain). The target antibiotics were chosen on the basis of a preliminary multispecies screening. The analysis of the antibiotics was carried out by LC-MS/MS on wastewater-treatment plant (WWTP) effluent, effluents of a slaughterhouse and hospital, rivers downstream and upstream of these WWTPs, and rivers close to extensive farming areas. The ANOVA test was performed to study the significant differences between the points exposed to concrete emission sources and antibiotic concentration. The monitoring, carried out from 2018 to 2020, has been essential to illustrating the presence of the most abundant antibiotics that were detected in the Ebro River basin. Enrofloxacin has appeared in river waters in significant concentrations, especially near intensive farming, meanwhile azithromycin has been frequently detected in wastewaters.

A method based on UPLC-MS/MS (ultraperformance liquid chromatography—tandem mass spectrometry) was optimized for the analysis of a broad set of antibiotics and their metabolites in surface and wastewaters after their preconcentration by solid-phase extraction (SPE). The method was applied to the monitoring of the river basin of the POCTEFA (Interregional Programme Spain-France-Andorra) territory (Spain and France) in frame of a sampling campaign (2020–2021) including 40 sampling points, 28 of them corresponding to surface waters and 12 to wastewaters. In total, 21 antibiotics belonging to different families, i.e., ciprofloxacin, sulfamethoxazole, trimethoprim, azithromycin, and their metabolites were detected. A higher overall antibiotic contamination was observed in the Spanish part of the POCTEFA territory. Several metabolites of the target antibiotics, some of them supposed to be more toxic than their parent compounds, were identified in the entire sampling network. Fluoroquinolones and sulfamethoxazole, as well as their metabolites, presented the highest detection frequency both in wastewaters and surface waters, and, consequently, should be considered as target compounds in the monitoring of the water resources of the POCTEFA territory.

The increasing presence of antibiotics such as cephalosporins in wastewater represents a significant environmental risk. These compounds are excreted in large quantities, and conventional wastewater treatment plants are often ineffective at their removal. Consequently, the development of more sustainable and efficient treatment technologies is essential. In this study, the removal of cephalosporins from aqueous solutions was evaluated through adsorption using pine bark biochar, photocatalysis with TiO₂, and a combination of both processes. Kinetic experiments were conducted with cephalosporin solutions (15 mg/L), employing 150 mg/L of biochar, 100 mg/L TiO₂, or their combination, under continuous stirring and/or UV-vis irradiation. Samples were collected at 0 and 120 min and analyzed via UV-vis spectrophotometry. Adsorption isotherms were established for initial cephalosporin concentrations ranging from 5 to 50 mg/L. The biochar alone achieved a removal efficiency of 94.2% after 120 min. Photocatalysis with TiO₂ alone resulted in 75% removal, while the combined approach reached 95.9%, indicating a synergistic effect between adsorption and photodegradation mechanisms. Kinetic data fitted the pseudo-second-order model, and the Langmuir isotherm provided the best correlation, suggesting monolayer adsorption. These findings demonstrate that pine bark biochar, whether used independently or in combination with TiO₂, constitutes an eco-friendly, effective, and low-cost alternative for the removal of antibiotics from wastewater, while simultaneously contributing to the valorization of forestry residues.