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

## TL;DR

The paper introduces a new, efficient method for detecting harmful PAH pollutants in water using a combination of extraction and fluorescence detection, meeting regulatory standards.

## Contribution

A validated solvent-efficient SBSE–HPLC–FLD method for detecting six PAHs in water matrices with sub-10 ng·L−1 limits using fluorescence detection alone.

## Key findings

- The method achieved detection limits of 0.4–1.8 ng·L−1 and matrix-verified LOQs of 1.5–10.9 ng·L−1.
- The procedure met EU Drinking Water Directive requirements for benzo[a]pyrene and regulated PAH sum.
- The method is cost-effective and suitable for routine compliance and surveillance in regulatory labs.

## Abstract

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.

The online version contains supplementary material available at 10.1007/s00244-026-01183-8.