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Determination of ketamine and norketamine in hair samples by µ-QuEChERS and gas chromatography coupled to tandem mass spectrometry

2025Artigo científico Acesso aberto
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dc.contributor.authorPelixo, Rodrigo
dc.contributor.authorBarroso, Mário
dc.contributor.authorRosado, Tiago
dc.contributor.authorGallardo, Eugenia
dc.date.accessioned2026-01-29T15:25:56Z
dc.date.available2026-01-29T15:25:56Z
dc.date.issued2025
dc.description.abstractKetamine has gained popularity in Europe as a new psychoactive substance due to its dissociative effects, which are sought after by users at raves, for unprescribed treatment of psychological issues, and in drug-facilitated crimes. Forensic experts often face challenges in proving drug use, and hair offers distinct advantages as a sample, revealing both long-term consumption and recent abuse. However, due to its complex nature, hair requires pretreatment to remove interferences and enhance analytical sensitivity. This study employs a miniaturised version of the “Quick, Easy, Cheap, Rugged, and Safe” (QuEChERS) extraction method, commonly used in food and environmental analyses. The method uses 1 mL of 5 % formic acid in acetonitrile and 250 mg ammonium formate as solvent and salt partitioning agents, along with 50 mg magnesium sulphate and 10 mg primary-secondary amine for dispersive solid-phase extraction. After this clean-up process, samples were analysed using gas chromatography coupled with tandem mass spectrometry. Following optimisation, the method was validated for detecting ketamine and its primary metabolite, norketamine. A limit of detection of 0.01 ng/mg was achieved for ketamine, and 0.8 ng/mg for norketamine, with limits of quantification of 0.05 ng/mg and 0.8 ng/mg, respectively. This established a working range of 0.05–5 ng/mg for ketamine and 0.8–5 ng/mg for norketamine. Recovery rates ranged from 47–76 % for ketamine and 14–27 % for norketamine. The method was then applied to real samples from drug users, proving the effectiveness of the µ-QuEChERS technique as a sustainable clean-up method. Despite its miniaturisation, it retained the performance of the original QuEChERS protocol and allowed obtaining high sensitivity, enabling analyte detection at a concentration below the Society of Hair Testing’s cut-off value of 0.2 ng/mg.eng
dc.identifier.citationPelixo, R., Barroso, M., Rosado, T., & Gallardo, E. (2025). Determination of ketamine and norketamine in hair samples by µ-QuEChERS and gas chromatography coupled to tandem mass spectrometry. Microchemical Journal, 213.
dc.identifier.doi10.1016/j.microc.2025.113770
dc.identifier.urihttp://hdl.handle.net/10400.26/61307
dc.language.isoeng
dc.peerreviewedyes
dc.publisherElsevier
dc.relationHealth Sciences Research Centre
dc.relationHealth Sciences Research Centre
dc.rights.urihttp://creativecommons.org/licenses/by/4.0/
dc.subjectQuEChERS
dc.subjectHair
dc.subjectKetamine
dc.subjectNorketamine
dc.titleDetermination of ketamine and norketamine in hair samples by µ-QuEChERS and gas chromatography coupled to tandem mass spectrometryeng
dc.typejournal article
dspace.entity.typePublication
oaire.awardTitleHealth Sciences Research Centre
oaire.awardTitleHealth Sciences Research Centre
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/6817 - DCRRNI ID/UIDB%2F00709%2F2020/PT
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/6817 - DCRRNI ID/UIDP%2F00709%2F2020/PT
oaire.citation.titleMicrochemical Journal
oaire.citation.volume213
oaire.fundingStream6817 - DCRRNI ID
oaire.fundingStream6817 - DCRRNI ID
oaire.versionhttp://purl.org/coar/version/c_970fb48d4fbd8a85
person.familyNameBarroso
person.familyNameRosado
person.familyNameGallardo
person.givenNameMário
person.givenNameTiago
person.givenNameEugenia
person.identifier.ciencia-id5110-F476-ECCC
person.identifier.ciencia-idC21B-DCC7-1C44
person.identifier.ciencia-idF617-5CA5-EF61
person.identifier.orcid0000-0001-8848-2734
person.identifier.orcid0000-0003-0469-2895
person.identifier.orcid0000-0002-1802-8998
person.identifier.scopus-author-id35329243100
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
relation.isAuthorOfPublication294b555e-48c4-4013-b981-b8917400c56c
relation.isAuthorOfPublication9ed79380-fe93-47d7-bc88-2bff71439695
relation.isAuthorOfPublicationdde2079f-5556-4f43-8253-77bd51c001fe
relation.isAuthorOfPublication.latestForDiscovery294b555e-48c4-4013-b981-b8917400c56c
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