Publicação
Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices
| Resumo: | 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 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. |
|---|---|
| Autores principais: | Fernandes-Lage, Eduardo |
| Outros Autores: | Alves, Maria José; Moura, Cosme; Garcia, Juliana |
| Assunto: | Polycyclic aromatic-hydrocarbons Bar sorptive extraction Performance liquid-chromatography Solid-phase extraction Gas-chromatography Fluorescence detection Combination |
| Ano: | 2026 |
| País: | Portugal |
| Tipo de documento: | artigo |
| Tipo de acesso: | acesso aberto |
| Instituição associada: | Instituto Politécnico de Bragança |
| Idioma: | inglês |
| Origem: | Biblioteca Digital do IPB |
| _version_ | 1867173416229928960 |
|---|---|
| author | Fernandes-Lage, Eduardo |
| author2 | Alves, Maria José Moura, Cosme Garcia, Juliana |
| author2_role | author author author |
| author_facet | Fernandes-Lage, Eduardo Alves, Maria José Moura, Cosme Garcia, Juliana |
| author_role | author |
| contributor_name_str_mv | Biblioteca Digital do IPB |
| country_str | PT |
| creators_json_txt | [{\"Person.name\":\"Fernandes-Lage, Eduardo\"},{\"Person.name\":\"Alves, Maria José\",\"Person.identifier.orcid\":\"0000-0001-8506-4393\"},{\"Person.name\":\"Moura, Cosme\"},{\"Person.name\":\"Garcia, Juliana\",\"Person.identifier.orcid\":\"0000-0002-3435-577X\"}] |
| datacite.contributors.contributor.contributorName.fl_str_mv | Biblioteca Digital do IPB |
| datacite.creators.creator.creatorName.fl_str_mv | Fernandes-Lage, Eduardo Alves, Maria José Moura, Cosme Garcia, Juliana |
| datacite.date.Accepted.fl_str_mv | 2026-01-01T00:00:00Z |
| datacite.date.available.fl_str_mv | 2026-02-25T09:36:38Z |
| datacite.date.embargoed.fl_str_mv | 2026-02-25T09:36:38Z |
| datacite.rights.fl_str_mv | http://purl.org/coar/access_right/c_abf2 |
| datacite.subjects.subject.fl_str_mv | Polycyclic aromatic-hydrocarbons Bar sorptive extraction Performance liquid-chromatography Solid-phase extraction Gas-chromatography Fluorescence detection Combination |
| datacite.titles.title.fl_str_mv | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices |
| dc.contributor.none.fl_str_mv | Biblioteca Digital do IPB |
| dc.creator.none.fl_str_mv | Fernandes-Lage, Eduardo Alves, Maria José Moura, Cosme Garcia, Juliana |
| dc.date.Accepted.fl_str_mv | 2026-01-01T00:00:00Z |
| dc.date.available.fl_str_mv | 2026-02-25T09:36:38Z |
| dc.date.embargoed.fl_str_mv | 2026-02-25T09:36:38Z |
| dc.format.none.fl_str_mv | application/pdf |
| dc.identifier.none.fl_str_mv | http://hdl.handle.net/10198/35849 |
| dc.language.none.fl_str_mv | eng |
| dc.publisher.none.fl_str_mv | Springer |
| dc.rights.cclincense.fl_str_mv | http://creativecommons.org/licenses/by-nc/4.0/ |
| dc.rights.none.fl_str_mv | http://purl.org/coar/access_right/c_abf2 |
| dc.subject.none.fl_str_mv | Polycyclic aromatic-hydrocarbons Bar sorptive extraction Performance liquid-chromatography Solid-phase extraction Gas-chromatography Fluorescence detection Combination |
| dc.title.fl_str_mv | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices |
| dc.type.none.fl_str_mv | http://purl.org/coar/resource_type/c_6501 |
| description | 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 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. |
| dirty | 0 |
| eu_rights_str_mv | openAccess |
| format | article |
| fulltext.url.fl_str_mv | https://bibliotecadigital.ipb.pt/bitstreams/50c1c49b-9888-42d5-a166-2c50b160f71d/download |
| funding.funder.alternateName_str_mv | FCT |
| funding.funder.identifier_str_mv | http://doi.org/10.13039/501100001871 |
| funding.funder.name_str_mv | Fundação para a Ciência e a Tecnologia |
| funding.name_str_mv | 6817 - DCRRNI ID |
| id | ipb_7abdfefdf0596853843db79eaf335437 |
| identifier.url.fl_str_mv | http://hdl.handle.net/10198/35849 |
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| institution | Instituto Politécnico de Bragança |
| instname_str | Instituto Politécnico de Bragança |
| language | eng |
| network_acronym_str | ipb |
| network_name_str | Biblioteca Digital do IPB |
| oai_identifier_str | oai:bibliotecadigital.ipb.pt:10198/35849 |
| organization_str_mv | urn:organizationAcronym:ipb |
| person_str_mv | Fernandes-Lage, Eduardo Alves, Maria José Alves, Maria José https://www.ciencia-id.pt/D618-B3A9-D312 D618-B3A9-D312 http://orcid.org/0000-0001-8506-4393 0000-0001-8506-4393 Moura, Cosme Garcia, Juliana Garcia, Juliana http://orcid.org/0000-0002-3435-577X 0000-0002-3435-577X |
| publishDate | 2026 |
| publisher.none.fl_str_mv | Springer |
| reponame_str | Biblioteca Digital do IPB |
| repository_id_str | urn:repositoryAcronym:ipb |
| service_str_mv | urn:repositoryAcronym:ipb |
| spelling | engSpringerengPolycyclic 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.application/pdfengOptimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water MatricesFernandes-Lage, EduardoPersonalAlves, Maria JoséDSpacehttp://dspace.org/items/7850f8c2-8834-4d5a-b4a7-df482abd76d3DSpacehttp://dspace.org/items/7850f8c2-8834-4d5a-b4a7-df482abd76d3AlvesMaria JoséCiência IDhttps://www.ciencia-id.ptD618-B3A9-D312ORCIDhttp://orcid.org0000-0001-8506-4393Researcher IDhttps://www.researcherid.comM-6624-2016Scopus Author IDhttps://www.scopus.com16400584800Moura, CosmePersonalGarcia, JulianaDSpacehttp://dspace.org/items/65122e77-80d7-4c77-b075-f6215956ae10DSpacehttp://dspace.org/items/65122e77-80d7-4c77-b075-f6215956ae10GarciaJulianaORCIDhttp://orcid.org0000-0002-3435-577XHostingInstitutionOrganizationalBiblioteca Digital do IPBe-mailmailto:dspace@ipb.ptdspace@ipb.ptISSNIsPartOf0090-4341ISSNIsPartOf1432-0703DOIIsPartOf10.1007/s00244-026-01183-82026-02-25T09:36:38Z20262026-01-01T00:00:00ZHandlehttp://hdl.handle.net/10198/35849http://purl.org/coar/access_right/c_abf2open accessPolycyclic aromatic-hydrocarbonsBar sorptive extractionPerformance liquid-chromatographySolid-phase extractionGas-chromatographyFluorescence detectionCombination3017557 bytesFundação para a Ciência e a TecnologiaAssociate Laboratory for Sustainability and Tecnology in Mountain Regions6817 - DCRRNI IDCrossref Funder IDhttp://doi.org/10.13039/501100001871literaturehttp://purl.org/coar/resource_type/c_6501journal article2026http://creativecommons.org/licenses/by-nc/4.0/http://purl.org/coar/access_right/c_abf2application/pdffulltexthttps://bibliotecadigital.ipb.pt/bitstreams/50c1c49b-9888-42d5-a166-2c50b160f71d/downloadArchives of Environmental Contamination and Toxicology902120 |
| spellingShingle | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices Fernandes-Lage, Eduardo Polycyclic aromatic-hydrocarbons Bar sorptive extraction Performance liquid-chromatography Solid-phase extraction Gas-chromatography Fluorescence detection Combination |
| status | SINGLETON |
| subject.fl_str_mv | Polycyclic aromatic-hydrocarbons Bar sorptive extraction Performance liquid-chromatography Solid-phase extraction Gas-chromatography Fluorescence detection Combination |
| title | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices |
| title_full | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices |
| title_fullStr | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices |
| title_full_unstemmed | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices |
| title_short | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices |
| title_sort | Optimization and Validation of the SBSE–HPLC–FLD Method for the Determination of Priority Pollutants PAHs in Several Water Matrices |
| topic | Polycyclic aromatic-hydrocarbons Bar sorptive extraction Performance liquid-chromatography Solid-phase extraction Gas-chromatography Fluorescence detection Combination |
| topic_facet | Polycyclic aromatic-hydrocarbons Bar sorptive extraction Performance liquid-chromatography Solid-phase extraction Gas-chromatography Fluorescence detection Combination |
| url | http://hdl.handle.net/10198/35849 |
| visible | 1 |