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Determination of Ketamine and Norketamine in hair samples using MEPS as sample clean-up

dc.contributor.authorSimão, Ana Y.
dc.contributor.authorOliveira, Patrik
dc.contributor.authorRosendo, Luana M.
dc.contributor.authorRosado, Tiago
dc.contributor.authorGallardo, Eugenia
dc.contributor.authorAndraus, Maristela
dc.contributor.authorBarroso, Mário
dc.date.accessioned2023-03-13T14:49:20Z
dc.date.available2023-03-13T14:49:20Z
dc.date.issued2022-06
dc.descriptionPalestra realizada no encontro SoHT-GTFI Joint Meeting, Verona, Junho 2022pt_PT
dc.description.abstractIntroduction and Aim: The use of hair samples to determine ketamine (K) and its metabolite, norketamine (NK), has been studied by several authors, using different clean-up approaches. However, microextraction by packed sorbent (MEPS), a miniaturized form of the classic solid-phase extraction has not been applied to date for the purpose. Therefore, a method to determine K and NK in hair samples was developed, optimized, and validated using MEPS as sample clean-up. Materials & Methods: Hair samples were scissor-cut into small fragments, and rinsed with methanol to remove dirt and externally deposited material. Following an overnight incubation with methanol at 65 ºC (no stirring), the compounds were analysed by GC-MS/MS without the need of derivatization procedures; MEPS conditions were: conditioning (5 x 250 µL of methanol and 4 x 250 µL of deionized water); load (10 x 150 µL of hair extract); washing (50 µL of 0.1% acetic acid and 50 µL of 10% methanol); and elution (100 µL of 3% ammonium hydroxide in methanol). Results & Discussion: The procedure resulted in acceptable recoveries, 39-61% for K and 32-43% for NK, and allowed reaching limits of quantification (LOQs) of 50 pg/mg for both analytes. The analytical method presented acceptable accuracy and precision with coefficients of variation typically lower than 15% and BIAS within ± 15%, except at the LOQ (20%). The method was successfully applied to 2 authentic samples, and ketamine concentrations were below 0.05 and 0.18 ng/mg. Norketamine was not detected. Conclusions: This work is the first analytical method using MEPS coupled to GC-MS/MS for the determination of K and NK in hair samples. Following a comparison with a SPE-based method using authentic samples, it was considered rapid and suitable for routine analysis. Acknowledgments: FCT (UIDB /00709/2020 and UIDP/00709/2020). A.Y. Simão acknowledges the PhD fellowship from FCT (2020.09070.BD).pt_PT
dc.description.versionN/Apt_PT
dc.identifier.urihttp://hdl.handle.net/10400.26/44097
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.relationHealth Sciences Research Centre
dc.relationHealth Sciences Research Centre
dc.subjectKetaminept_PT
dc.subjectHairpt_PT
dc.subjectMEPSpt_PT
dc.titleDetermination of Ketamine and Norketamine in hair samples using MEPS as sample clean-uppt_PT
dc.typelecture
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.awardURIinfo:eu-repo/grantAgreement/FCT/POR_CENTRO/2020.09070.BD/PT
oaire.citation.conferencePlaceVerona (Italy)pt_PT
oaire.citation.titleSoHT-GTFI Joint Meetingpt_PT
oaire.fundingStream6817 - DCRRNI ID
oaire.fundingStream6817 - DCRRNI ID
oaire.fundingStreamPOR_CENTRO
person.familyNameSimão
person.familyNameOliveira
person.familyNameda Silva Rosendo
person.familyNameRosado
person.familyNameGallardo
person.familyNameAndraus
person.familyNameBarroso
person.givenNameAna Aysa
person.givenNamePatrik
person.givenNameLuana May
person.givenNameTiago
person.givenNameEugenia
person.givenNameMaristela
person.givenNameMário
person.identifier.ciencia-id4E12-377B-7569
person.identifier.ciencia-idC21B-DCC7-1C44
person.identifier.ciencia-idF617-5CA5-EF61
person.identifier.ciencia-id5110-F476-ECCC
person.identifier.orcid0000-0003-3199-1866
person.identifier.orcid0000-0002-2517-7801
person.identifier.orcid0000-0002-0461-8540
person.identifier.orcid0000-0003-0469-2895
person.identifier.orcid0000-0002-1802-8998
person.identifier.orcid0000-0002-6611-0443
person.identifier.orcid0000-0001-8848-2734
person.identifier.scopus-author-id57218392172
person.identifier.scopus-author-id35329243100
project.funder.identifierhttp://doi.org/10.13039/501100001871
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
project.funder.nameFundação para a Ciência e a Tecnologia
rcaap.rightsopenAccesspt_PT
rcaap.typelecturept_PT
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