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Analysis of organophosphorus pesticides in whole blood by GC-MS-μECD with forensic purposes

dc.contributor.authorValente, Nuno I.P.
dc.contributor.authorTarelho, Sónia
dc.contributor.authorCastro, André Lobo
dc.contributor.authorSilvestre, Armando
dc.contributor.authorTeixeira, Helena M.
dc.date.accessioned2023-02-17T16:10:45Z
dc.date.available2023-02-17T16:10:45Z
dc.date.issued2015-03-28
dc.description.abstractIn the present work, two multi-residue methods for the determination of ten organophosphorus pesticides (OPs), namely chlorfenvinphos, chlorpyrifos, diazinon, dimethoate, fenthion, malathion, parathion, phosalone, pirimiphos-methyl and quinalphos, in post-mortem whole blood samples are presented. The adopted procedure uses GC-MS for screening and quantitation, and GC-µECD (electron capture detector) for compound confirmation. Three different Solid Phase Extraction (SPE) procedures for OPs with Oasis® hydrophilic lipophilic balanced (HLB) and Sep-Pak® C18 cartridges were tested, and followed by GC-µECD and GC-MS analysis. The Sep-Pak® C18 cartridges extraction procedure was selected since it generated analytical signals 5 times higher than those obtained with the two different Oasis® HLB cartridges extraction procedures. The method has shown to be selective for the isolation of selected OPs as well as to the chosen internal standard (ethion) in postmortem blood samples. Calibration curves between 50 and 5000 ng/mL were prepared using weighted linear regression models (1/x2). It was not possible to establish a working range for fenthion by GC-µECD due to the lower sensitivity of the detector to this compound, whereas for pirimiphos-methyl it was set between 500 and 5000 ng/mL. The limit of quantitation was established at 50 ng/mL for all analytes, except for pirimiphos-methyl by GC-µECD analysis (500 ng/mL). The average extraction efficiency ranged from 72 to 102%. The developed methods were considered robust and fit for the purpose, and had already been adopted in the laboratory routine analysis.pt_PT
dc.description.versioninfo:eu-repo/semantics/acceptedVersionpt_PT
dc.identifier.citationValente NIP, Tarelho S, Castro AL, Silvestre A, Teixeira HM, “Analysis of organophosphorus pesticides in whole blood by GC-MS-mECD with forensic purposes”, Journal of Forensic and Legal Medicine, 33 (2015) 28-34.pt_PT
dc.identifier.doi10.1016/j.jflm.2015.03.006pt_PT
dc.identifier.urihttp://hdl.handle.net/10400.26/43905
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherElsevierpt_PT
dc.relationCICECO-Aveiro Institute of Materials
dc.rights.urihttp://creativecommons.org/licenses/by-nc-nd/4.0/pt_PT
dc.subjectGC-MS-ECDpt_PT
dc.subjectAnalytical method validationpt_PT
dc.subjectOrganophosphorus pesticidespt_PT
dc.subjectPost-mortem blood samplespt_PT
dc.subjectSPE Sep-Pak C18 cartridgespt_PT
dc.titleAnalysis of organophosphorus pesticides in whole blood by GC-MS-μECD with forensic purposespt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.awardTitleCICECO-Aveiro Institute of Materials
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/6817 - DCRRNI ID/UID%2FCTM%2F50011%2F2013/PT
oaire.citation.endPage34pt_PT
oaire.citation.startPage28pt_PT
oaire.citation.titleJournal of Forensic and Legal Medicinept_PT
oaire.citation.volume33pt_PT
oaire.fundingStream6817 - DCRRNI ID
person.familyNameValente
person.familyNameTarelho
person.familyNameLobo Castro
person.familyNameDomingues Silvestre
person.familyNameTeixeira
person.givenNameNuno I.P.
person.givenNameSónia
person.givenNameAndré
person.givenNameArmando Jorge
person.givenNameHelena M.
person.identifierE-6201-2010
person.identifier.ciencia-idDC18-EB22-B357
person.identifier.ciencia-id4214-85EB-E58C
person.identifier.orcid0000-0001-7003-1628
person.identifier.orcid0000-0001-8366-6702
person.identifier.orcid0000-0002-7258-8523
person.identifier.orcid0000-0001-5403-8416
person.identifier.orcid0000-0001-7570-5521
person.identifier.scopus-author-id7005219944
person.identifier.scopus-author-id7003981256
project.funder.identifierhttp://doi.org/10.13039/501100001871
project.funder.nameFundação para a Ciência e a Tecnologia
rcaap.rightsopenAccesspt_PT
rcaap.typearticlept_PT
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