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Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices

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Resumo:Polycyclic aromatic hydrocarbons (PAHs) are priority pollutants in drinking and environmental waters. Their mutagenic/carcinogenic potential and ng.L-1 limits demand methods that are both sensitive and practical. We report a rapid, solvent-sparing workflow coupling stir-bar sorptive extraction (SBSE) to HPLC with fluorescence detection (FLD) for simultaneous determination of six PAHs (fluoranthene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, benzo[ghi]perylene, indeno[1,2,3-cd]pyrene) in drinking water, groundwater, and surface water. SBSE conditions were optimized, and isocratic RP-HPLC achieved baseline resolution within a 26-min cycle using similar to 39 mL solvent (similar to 20 samples day - 1). Validation under ISO/IEC 17,025 showed linear calibration (r >= 0.99941), limits of detection of 0.4-1.8 ng.L-1, and matrix-verified LOQs of 1.5-10.9 ng.L-1. Trueness and precision met predefined criteria across matrices (recoveries 63.3-109.9%; within-laboratory reproducibility <= 25% RSD), with expanded uncertainties U(k = 2) <= 47.1%. Performance satisfies EU Drinking Water Directive 2020/2184 requirements for benzo[a]pyrene and the regulated PAH sum. By attaining sub-10 ng.L-1 LOQs with FLD alone and documenting a complete uncertainty budget, this procedure offers a cost-effective alternative to LC-MS/MS for routine compliance and surveillance. The validated SBSE-HPLC-FLD protocol is fit-for-purpose for regulatory laboratories and environmental services requiring sensitive, robust, and scalable PAH determination across diverse water matrices.
Autores principais:Fernandes-Lage, Eduardo
Outros Autores:Alves, Maria José; Moura, Cosme; Garcia, Juliana
Assunto:Polycyclic aromatic-hydrocarbons Bar sorptive extraction Performance liquid-chromatography Solid-phase extraction Gas-chromatography Fluorescence detection Combination
Ano:2026
País:Portugal
Tipo de documento:artigo
Tipo de acesso:acesso aberto
Instituição associada:Instituto Politécnico de Bragança
Idioma:inglês
Origem:Biblioteca Digital do IPB

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