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Extraction of pesticides from soil using direct-immersion SPME LC-Tips followed by GC–MS/MS

dc.contributor.authorBrinco, João
dc.contributor.authorCarvalho, Raquel
dc.contributor.authorSilva, Marco Gomes da
dc.contributor.authorGuedes, Paula
dc.contributor.authorRibeiro, Alexandra B.
dc.contributor.authorMateus, Eduardo P.
dc.contributor.institutionDCEA - Departamento de Ciências e Engenharia do Ambiente
dc.contributor.institutionLAQV@REQUIMTE
dc.contributor.institutionDQ - Departamento de Química
dc.contributor.institutionCENSE - Centro de Investigação em Ambiente e Sustentabilidade
dc.contributor.pblElsevier Science B.V., Amsterdam.
dc.date.accessioned2025-02-25T22:06:26Z
dc.date.available2025-02-25T22:06:26Z
dc.date.issued2024-10
dc.descriptionLAQV/REQUIMTE (UID/QUI/50006/2020). UI/BD/150867/2021. CEECIND/01969/2020. © 2024 The Author(s). Published by Elsevier B.V.
dc.description.abstractA new method was evaluated and developed for the analysis of pesticides in sandy-loam soil by direct-immersion solid phase microextraction (DI-SPME) followed by gas chromatography tandem-mass spectrometry (GC–MS/MS) determination. Ten pesticides were selected based on a literature survey of the compounds reported to be present in EU soils. The extraction was performed using SPME LC-Tips, a new SPME configuration with the coated fibers attached to a disposable and easy-to-handle micropipette tip, which was immersed into a soil slurry made by the addition of an aqueous solution to the soil sample. Ten experimental parameters were evaluated with a Plackett-Burman design, after which the extraction time and percentage of organic solvent in the aqueous extraction were optimized separately. The two fiber chemistries available (PDMS/DVB and C18) were evaluated in parallel for the entire work. In the final method, slurry samples were made by adding an aqueous solution (6 % methanol v/v) to 2 g of soil. The fiber was conditioned and then inserted, for extraction, into the samples, stirred by a magnetic bar. Afterwards, the analytes were desorbed onto 100 µL of methanol. After the addition of analyte protectants (ethylglycerol, gulonolactone, and sorbitol) the extract was injected into the GC–MS/MS system. Isotopically labelled penconazole was used as internal standard. A calibration was performed by extracting spiked soil with analyte concentrations of 0.1–50 µg/kg. Coefficients of determination of the linear calibration were between 0.94–0.98 for the PDMS/DVB and 0.92–0.99 for the C18. Limits of detection range between 0.01–10 µg/kg for the PDMS/DVB and 0.1–10 µg/kg for the C18. Overall, the C18 analytically outperformed the PDMS/DVB but required a longer extraction time (120 min vs 75 min for the PDMS/DVB). This method allows automation and generates low residual toxic waste, having the potential to be introduced as a greener and simpler alternative to currently used sample preparation methodologies.en
dc.description.versionpublishersversion
dc.description.versionpublished
dc.format.extent2072223
dc.identifier.doi10.1016/j.chroma.2024.465295
dc.identifier.issn0021-9673
dc.identifier.otherPURE: 104658489
dc.identifier.otherPURE UUID: dc68207d-7a96-4ec7-b652-992796eb1a53
dc.identifier.otherORCID: /0000-0003-1761-7376/work/166794378
dc.identifier.otherWOS: 001308245700001
dc.identifier.otherPubMed: 39236359
dc.identifier.otherScopus: 85203013949
dc.identifier.otherORCID: /0000-0002-5606-3591/work/178935817
dc.identifier.urihttp://hdl.handle.net/10362/179814
dc.identifier.urlhttps://www.scopus.com/pages/publications/85203013949
dc.language.isoeng
dc.peerreviewedyes
dc.relationinfo:eu-repo/grantAgreement/FCT/Concurso para Financiamento de Projetos de Investigação Científica e Desenvolvimento Tecnológico em Todos os Domínios Científicos - 2020/PTDC%2FCTA-AMB%2F6587%2F2020/PT
dc.relationinfo:eu-repo/grantAgreement/FCT//UI%2FBD%2F150867%2F2021/PT
dc.relationPesticide soil pollution: electrokinetic remediation, advanced monitoring tools and degradation mechanisms
dc.subjectAnalysis
dc.subjectDirect immersion SPME
dc.subjectPesticide
dc.subjectSoil
dc.subjectsoil pesticide extraction
dc.titleExtraction of pesticides from soil using direct-immersion SPME LC-Tips followed by GC–MS/MSen
dc.title.subtitleEvaluation and proof-of-concepten
dc.typejournal article
degois.publication.titleJournal Of Chromatography A
degois.publication.volume1735
dspace.entity.typePublication
oaire.awardNumberPTDC/CTA-AMB/6587/2020
oaire.awardNumberUI/BD/150867/2021
oaire.awardTitlePesticide soil pollution: electrokinetic remediation, advanced monitoring tools and degradation mechanisms
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/Concurso para Financiamento de Projetos de Investigação Científica e Desenvolvimento Tecnológico em Todos os Domínios Científicos - 2020/PTDC%2FCTA-AMB%2F6587%2F2020/PT
oaire.awardURIinfo:eu-repo/grantAgreement/FCT//UI%2FBD%2F150867%2F2021/PT
oaire.fundingStreamConcurso para Financiamento de Projetos de Investigação Científica e Desenvolvimento Tecnológico em Todos os Domínios Científicos - 2020
project.funder.identifierhttp://doi.org/10.13039/501100001871
project.funder.identifierhttp://doi.org/10.13039/501100001871
project.funder.nameFundação para a Ciência e a Tecnologia
project.funder.nameFundação para a Ciência e a Tecnologia
rcaap.rightsopenAccess
relation.isProjectOfPublication1c6fb545-6a93-48f4-b184-7fd5b1e5e60e
relation.isProjectOfPublication7493c5e7-ff04-4f8c-b222-9586524db720
relation.isProjectOfPublication.latestForDiscovery1c6fb545-6a93-48f4-b184-7fd5b1e5e60e

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