An Efficient and Greener Alternative for the Extraction of Polycyclic Aromatic Compounds from Sediments

This study details the validation of a novel microbead beating extraction (MBE) technique for the analysis of polycyclic aromatic compounds (PACs) in sediments. The method’s performance was evaluated against international analytical validation criteria, including trueness, precision, measurement uncertainty and robustness. Limits of detection and quantitation were consistently low (≤6.5 and 21 ng g−1, respectively), trueness for the majority of analytes fell within accepted performance criteria, and repeatability values for most analytes were generally <10%. Analytical data confirm the method’s reliability, with more than 80% of certified analytes in two certified reference materials (CRMs) meeting the satisfactory z-score (∣z∣ ≤ 2.0). Furthermore, the method’s inter-laboratory repeatability, as measured by HorRat values, fell within the range recommended by the Association for Official Analytical Chemist for most analytes, and combined measurement uncertainties showed no statistical difference from the certified uncertainties of the CRMs. Incorporating an in situ cleanup step enabled the MBE method to substantially reduce extraction times (<15 min) and reduces solvent consumption by ~60% compared with conventional pressurize fluid extraction while maintaining good quality data objectives. By meeting or exceeding well-established metrics for good laboratory performance, the MBE method demonstrates reliability, efficiency, and a greener approach for the routine analysis of PACs in sediments.