A rapid and reliable method based on magnetic solid-phase extraction (MSPE) and ultra-high performance liquid chromatography (UHPLC-FLD) analysis was developed and validated for the quantitative determination of seven polycyclic aromatic hydrocarbons (PAHs) in water samples. Hybrid composites made up of magnetic nanoparticles (MNPs) and carbon nanotubes (CNTs) were tested as adsorbent materials. The main factors influencing the extraction yields were optimized, namely the amount and type of adsorbent in the adsorption, and the solvent, the type of energy and the time in the desorption step. The selected composite was made up of FeO and multiwalled (MW)-CNTs. The desorption was carried out with sonication probe and tetrahydrofuran (THF); this solvent makes the method directly compatible with the chromatographic mobile phase and it reduces the analysis time. Under the optimized conditions, the LODs and LOQs achieved were in the range of 0.025-0.73 and 0.04-2.4 ng mL, respectively. The calibration curves were linear (R ≥ 0.9936) over the concentration ranges from 1 to 500 ng mL. The recoveries of PAHs were from 76.4 ± 1.7 up to 106.5 ± 3.5%. The method was applied to synthetic and real (tap, dam, river and mineral) water samples with different characteristics to evaluate the performance under real conditions.
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