<p>Polycyclic aromatic hydrocarbons (PAHs) are priority pollutants in drinking and environmental waters. Their mutagenic/carcinogenic potential and ng·L<sup>− 1</sup> 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 ~ 39 mL solvent (~ 20 samples day − 1). Validation under ISO/IEC 17,025 showed linear calibration (<i>r</i> ≥ 0.99941), limits of detection of 0.4–1.8 ng·L<sup>− 1</sup>, and matrix-verified LOQs of 1.5–10.9 ng·L<sup>− 1</sup>. 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<sup>− 1</sup> 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.</p>

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

  • Eduardo Fernandes-Lage,
  • Maria José Alves,
  • Cosme Moura,
  • Juliana Garcia

摘要

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 ~ 39 mL solvent (~ 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.