Publicação
Extraction of pesticides from soil using direct-immersion SPME LC-Tips followed by GC–MS/MS
| dc.contributor.author | Brinco, João | |
| dc.contributor.author | Carvalho, Raquel | |
| dc.contributor.author | Silva, Marco Gomes da | |
| dc.contributor.author | Guedes, Paula | |
| dc.contributor.author | Ribeiro, Alexandra B. | |
| dc.contributor.author | Mateus, Eduardo P. | |
| dc.contributor.institution | DCEA - Departamento de Ciências e Engenharia do Ambiente | |
| dc.contributor.institution | LAQV@REQUIMTE | |
| dc.contributor.institution | DQ - Departamento de Química | |
| dc.contributor.institution | CENSE - Centro de Investigação em Ambiente e Sustentabilidade | |
| dc.contributor.pbl | Elsevier Science B.V., Amsterdam. | |
| dc.date.accessioned | 2025-02-25T22:06:26Z | |
| dc.date.available | 2025-02-25T22:06:26Z | |
| dc.date.issued | 2024-10 | |
| dc.description | LAQV/REQUIMTE (UID/QUI/50006/2020). UI/BD/150867/2021. CEECIND/01969/2020. © 2024 The Author(s). Published by Elsevier B.V. | |
| dc.description.abstract | A 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.version | publishersversion | |
| dc.description.version | published | |
| dc.format.extent | 2072223 | |
| dc.identifier.doi | 10.1016/j.chroma.2024.465295 | |
| dc.identifier.issn | 0021-9673 | |
| dc.identifier.other | PURE: 104658489 | |
| dc.identifier.other | PURE UUID: dc68207d-7a96-4ec7-b652-992796eb1a53 | |
| dc.identifier.other | ORCID: /0000-0003-1761-7376/work/166794378 | |
| dc.identifier.other | WOS: 001308245700001 | |
| dc.identifier.other | PubMed: 39236359 | |
| dc.identifier.other | Scopus: 85203013949 | |
| dc.identifier.other | ORCID: /0000-0002-5606-3591/work/178935817 | |
| dc.identifier.uri | http://hdl.handle.net/10362/179814 | |
| dc.identifier.url | https://www.scopus.com/pages/publications/85203013949 | |
| dc.language.iso | eng | |
| dc.peerreviewed | yes | |
| dc.relation | info: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.relation | info:eu-repo/grantAgreement/FCT//UI%2FBD%2F150867%2F2021/PT | |
| dc.relation | Pesticide soil pollution: electrokinetic remediation, advanced monitoring tools and degradation mechanisms | |
| dc.subject | Analysis | |
| dc.subject | Direct immersion SPME | |
| dc.subject | Pesticide | |
| dc.subject | Soil | |
| dc.subject | soil pesticide extraction | |
| dc.title | Extraction of pesticides from soil using direct-immersion SPME LC-Tips followed by GC–MS/MS | en |
| dc.title.subtitle | Evaluation and proof-of-concept | en |
| dc.type | journal article | |
| degois.publication.title | Journal Of Chromatography A | |
| degois.publication.volume | 1735 | |
| dspace.entity.type | Publication | |
| oaire.awardNumber | PTDC/CTA-AMB/6587/2020 | |
| oaire.awardNumber | UI/BD/150867/2021 | |
| oaire.awardTitle | Pesticide soil pollution: electrokinetic remediation, advanced monitoring tools and degradation mechanisms | |
| oaire.awardURI | info: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.awardURI | info:eu-repo/grantAgreement/FCT//UI%2FBD%2F150867%2F2021/PT | |
| oaire.fundingStream | Concurso para Financiamento de Projetos de Investigação Científica e Desenvolvimento Tecnológico em Todos os Domínios Científicos - 2020 | |
| project.funder.identifier | http://doi.org/10.13039/501100001871 | |
| project.funder.identifier | http://doi.org/10.13039/501100001871 | |
| project.funder.name | Fundação para a Ciência e a Tecnologia | |
| project.funder.name | Fundação para a Ciência e a Tecnologia | |
| rcaap.rights | openAccess | |
| relation.isProjectOfPublication | 1c6fb545-6a93-48f4-b184-7fd5b1e5e60e | |
| relation.isProjectOfPublication | 7493c5e7-ff04-4f8c-b222-9586524db720 | |
| relation.isProjectOfPublication.latestForDiscovery | 1c6fb545-6a93-48f4-b184-7fd5b1e5e60e |
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