Optimization and comparison of several extraction methods for determining perfluoroalkyl substances in soil matrices using liquid chromatography-mass spectrometry

Entity: Universitat Rovira i Virgili (URV)

Confidenciality: No

Education area(s): Tècniques Cromatogràfiques Aplicades

APS: No

Title in different languages: Optimization and comparison of several extraction methods for determining perfluoroalkyl substances in soil matrices using liquid chromatography-mass spectrometry

Abstract: Per- and polyfluoroalkyl substances (PFAS) are highly persistent synthetic chemicals recently classified as persistent organic pollutants (POPs) under the Stockholm Convention. They include both legacy compounds such as PFOS, PFOA, and PFHxS, and new-generation alternatives like HFPO-DA, DONA, and PFECHS. Soil acts as a key reservoir and secondary source of PFAS, yet analytical protocols for this matrix remain less developed compared with water, biota, or biosolids. This study evaluated and compared three extraction and clean-up strategies for PFAS determination in soils using UHPLC–MS/MS. The ENVI-Carb™ method, routinely applied in our laboratory, was assessed alongside an alternative cleanup with Oasis WAX/GCB cartridges and a QuEChERS-based protocol adapted from biological and environmental matrices. A naturally contaminated soil sample was analyzed, targeting 38 PFAS. The results showed clear differences between methods. The ENVI-Carb method provided acceptable precision but recovered only a limited subset of analytes, failing in particular to quantify some short-chain PFCAs such as PFBA. Oasis WAX/GCB achieved broader coverage and lower RSD values, combining acceptable recoveries with improved reproducibility. QuEChERS enabled the detection of the widest range of analytes, including certain long-chain PFAS associated with humic fractions, but overall recoveries were lower and RSD higher. Rather than selecting a single method as definitive, the results suggest two directions for future work: optimization of the QuEChERS protocol to reduce matrix interferences and improve recoveries, and the evaluation of the full Waters Oasis WAX/GC protocol, including its extraction step, to determine whether it can further enhance performance in soil matrices.

Subject: Espectrometria de masses

Academic year: 2024-2025

Language: en

Work's public defense date: 2025-09-10

Subject areas: Chemistry

Student: El Yaouti El Bouyakoubi, Kaoutar

Department: Química Analítica i Química Orgànica

Creation date in repository: 2025-11-26

Keywords: QuEChERS, matrices de suelo, SPE

Title in original language: Optimization and comparison of several extraction methods for determining perfluoroalkyl substances in soil matrices using liquid chromatography-mass spectrometry

Access Rights: info:eu-repo/semantics/openAccess

Project director: Marcé Recasens, Rosa Maria