RT Journal Article T1 Development of an analytical method for emerging contaminants including the pharmaceuticals recently selected as key performance indicators of the quaternary treatment of urban wastewater A1 Duque Villaverde, Andrés A1 Sóñora Otero, Sergio A1 Antonelli, Raissa A1 Vilar, Vítor J.P. A1 Carro Díaz, Antonia María A1 Dagnac, Thierry A1 Llompart Vizoso, María del Pilar K1 Emerging contaminants K1 Wastewater K1 Pharmaceuticals K1 6PPD-quinone K1 Solid-phase extraction K1 Liquid chromatography-mass spectrometry AB The revised European Directive concerning Urban Wastewater Treatment introduced the quaternary treatment for micropollutants. This directive lists 13 substances used as indicators of the performance of quaternary treatment, including pharmaceuticals such as antihypertensives and antidepressants, as well as some benzotriazoles. This article describes the development of an analytical method to determine these analytes and tire-related contaminants in wastewater and environmental samples. The method involves solid-phase extraction (SPE) followed by liquid chromatography coupled to tandem mass spectrometry (MS/MS) and high-resolution mass spectrometry (QTOF-HRMS). An experimental design is carried out to evaluate the influence of four factors affecting the extraction. Further studies were performed to achieve higher enrichment and thus lower detection limits. The method is validated in terms of analytical figures, and the matrix effect is assessed in water samples of different origins, demonstrating suitability. Real samples were analyzed showing the presence of some of the target compounds in natural waters (sea and river). In the wastewater samples, almost all the substances included in the directive, such as diclofenac, irbesartan or benzotriazole, were detected at levels up to 3 μg L−1. This method will help to assess the risks that the discharge of the targeted contaminants in urban wastewater poses for the environment and public health. PB Springer SN 1618-2642 YR 2025 FD 2025 LK https://hdl.handle.net/10347/43560 UL https://hdl.handle.net/10347/43560 LA eng NO Duque-Villaverde, A., Sóñora, S., Antonelli, R., Vilar, V. J.P., Carro, A.M., Dagnac, T., Llompart, M. (2025). Development of an analytical method for emerging contaminants including the pharmaceuticals recently selected as key performance indicators of the quaternary treatment of urban wastewater. Analytical and Bioanalytical Chemistry NO This research is part of the projects PID2022-140148OB-I00 and PID2022-139874OR-C22, funded by MICIU/AEI/10.13039/501100011033 and FEDER, EU, and is also supported by projects ED431B 2023/04 and IN607B 2022/15 (Xunta de Galicia). This work was financially supported by: UID/50020 of LSRE-LCM—Laboratory of Separation and Reaction Engineering – Laboratory of Catalysis and Materials—funded by Fundação para a Ciência e a Tecnologia, I.P./MCTES through national funds; and ALiCE, LA/P/0045/2020 (DOI:10.54499/LA/P/0045/2020). A.D. acknowledges Iacobus Program for his grant and Xunta de Galicia for his predoctoral contract (ED481A-2025-005). S.S. acknowledges the Ministry of Science, Innovation and Universities (Spain) for his predoctoral contract (PREP2022-000520). DS Minerva RD 24 abr 2026