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

2026Artigo científico Acesso aberto
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datacite.subject.fosEngenharia e Tecnologia::Engenharia Química
datacite.subject.fosEngenharia e Tecnologia::Engenharia do Ambiente
datacite.subject.sdg06:Água Potável e Saneamento
datacite.subject.sdg03:Saúde de Qualidade
dc.contributor.authorFernandes-Lage, Eduardo
dc.contributor.authorAlves, Maria José
dc.contributor.authorMoura, Cosme
dc.contributor.authorGarcia, Juliana
dc.date.accessioned2026-02-25T09:36:38Z
dc.date.available2026-02-25T09:36:38Z
dc.date.issued2026
dc.description.abstractPolycyclic 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.eng
dc.description.sponsorshipThis work is supported by National Funds by FCT –Portuguese Foundation for Science and Technology, under the projects UID/04033: Centro de Investigação e de Tecnologias Agro-Ambientais e Biológicas and LA/P/0126/2020 (https://doi.org/10.54499/LA/P/0126/2020 Juliana Garcia and Eduardo Lage acknowledge funding support from Portuguese public funding through Investimento RE-C05-i02 – Missão Interface N.° 01/C05-i02/2022.
dc.identifier.citationFernandes-Lage, Eduardo; Alves, Maria José; Moura, Cosme; Garcia, Juliana (2026). Optimization and Validation of the SBSE-HPLC-FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices. Archives of Environmental Contamination and Toxicology. ISSN 0090-4341. 90:2, p. 1-20
dc.identifier.doi10.1007/s00244-026-01183-8
dc.identifier.issn0090-4341
dc.identifier.issn1432-0703
dc.identifier.urihttp://hdl.handle.net/10198/35849
dc.language.isoeng
dc.peerreviewedyes
dc.publisherSpringer
dc.relationAssociate Laboratory for Sustainability and Tecnology in Mountain Regions
dc.relation.ispartofArchives of Environmental Contamination and Toxicology
dc.rights.urihttp://creativecommons.org/licenses/by-nc/4.0/
dc.subjectPolycyclic aromatic-hydrocarbons
dc.subjectBar sorptive extraction
dc.subjectPerformance liquid-chromatography
dc.subjectSolid-phase extraction
dc.subjectGas-chromatography
dc.subjectFluorescence detection
dc.subjectCombination
dc.titleOptimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matriceseng
dc.typejournal article
dspace.entity.typePublication
oaire.awardNumberLA/P/0007/2020
oaire.awardTitleAssociate Laboratory for Sustainability and Tecnology in Mountain Regions
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/6817 - DCRRNI ID/LA%2FP%2F0007%2F2020/PT
oaire.citation.endPage20
oaire.citation.issue2
oaire.citation.startPage1
oaire.citation.titleArchives of Environmental Contamination and Toxicology
oaire.citation.volume90
oaire.fundingStream6817 - DCRRNI ID
oaire.versionhttp://purl.org/coar/version/c_970fb48d4fbd8a85
person.familyNameAlves
person.familyNameGarcia
person.givenNameMaria José
person.givenNameJuliana
person.identifier.ciencia-idD618-B3A9-D312
person.identifier.orcid0000-0001-8506-4393
person.identifier.orcid0000-0002-3435-577X
person.identifier.ridM-6624-2016
person.identifier.scopus-author-id16400584800
project.funder.identifierhttp://doi.org/10.13039/501100001871
project.funder.nameFundação para a Ciência e a Tecnologia
relation.isAuthorOfPublication7850f8c2-8834-4d5a-b4a7-df482abd76d3
relation.isAuthorOfPublication65122e77-80d7-4c77-b075-f6215956ae10
relation.isAuthorOfPublication.latestForDiscovery7850f8c2-8834-4d5a-b4a7-df482abd76d3
relation.isProjectOfPublication6255046e-bc79-4b82-8884-8b52074b4384
relation.isProjectOfPublication.latestForDiscovery6255046e-bc79-4b82-8884-8b52074b4384

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