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Detection and quantification of selected cannabinoids in hair samples by liquid-liquid extraction and LC-MS/MS

dc.contributor.authorAntunes, Mónica
dc.contributor.authorSimões, Susana
dc.contributor.authorFonseca, Suzana
dc.contributor.authorFranco, João
dc.contributor.authorBarroso, Mário
dc.contributor.authorGallardo, Eugenia
dc.date.accessioned2026-04-20T17:29:06Z
dc.date.available2026-04-20T17:29:06Z
dc.date.issued2026-02
dc.description.abstractCannabis remains the most used illicit drug worldwide, with rising use linked to medical and recreational decriminalization. This has driven the development of analytical techniques to detect cannabinoids in biological matrices. Hair offers key advantages due to its non-invasive collection, extended detection window, stability, and easy storage. This study presents the development and validation of a robust method for extracting natural cannabinoids from hair, following ANSI/ASB 2019, FDA, and Society of Hair Testing guidelines. Hair samples were washed with methanol and cut into small pieces. Approximately 20 mg of hair was incubated with 1 M NaOH and methanol (30 min, 50 °C). The mixture was acidified with acetic acid and underwent liquid-liquid extraction using hexane/ethyl acetate (90/10, v/v). The organic phase was evaporated and reconstituted in 1-pentanol/methanol (50/50, v/v). Analysis was conducted by LC-MS/MS using multiple reaction monitoring (MRM) and triple-stage mass spectrometry (MS³). The method was selective, specific, precise, and linear, with working ranges of 5-2000 pg/mg for THC, CBN, and CBD; 50-2000 pg/mg for THC-OH; and 0.2-20 pg/mg for THC-COOH. Ion suppression was observed but did not affect sensitivity, with LLOQs and LODs from 0.2 to 50 pg/mg. Over 25 hair samples from university students tested positive for cannabis. THC ranged from 5.9 to 2430.7 pg/mg; one sample had THC-OH above LLOQ (61.4 pg/mg); THC-COOH ranged from 0.3 and 36.4 pg/mg; CBN from 5.7 to 461.0 pg/mg; and CBD from 5.7 to 850.2 pg/mg. Results aligned with self-reported use, confirming the method's forensic suitability.eng
dc.identifier.citationAntunes, M., Simões, S., Fonseca, S., Franco, J. M., Barroso, M., & Gallardo, E. (2026). Detection and quantification of selected cannabinoids in hair samples by liquid-liquid extraction and LC-MS/MS. Forensic science international, 378, 112685.
dc.identifier.doi10.1016/j.forsciint.2025.112685
dc.identifier.issn1872-6283
dc.identifier.urihttp://hdl.handle.net/10400.26/62809
dc.language.isoen
dc.peerreviewedyes
dc.publisherElsevier
dc.relationHealth Sciences Research Centre
dc.relationHealth Sciences Research Centre
dc.rights.urihttp://creativecommons.org/licenses/by/4.0/
dc.subjectCannabinoids
dc.subjectHair analysis
dc.subjectLC–MS/MS
dc.subjectMS(3)
dc.titleDetection and quantification of selected cannabinoids in hair samples by liquid-liquid extraction and LC-MS/MSeng
dc.typejournal article
dspace.entity.typePublication
oaire.awardNumberUIDB/00709/2020
oaire.awardNumberUIDP/00709/2020
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.issue378
oaire.citation.titleForensic Science International
oaire.fundingStream6817 - DCRRNI ID
oaire.fundingStream6817 - DCRRNI ID
oaire.versionhttp://purl.org/coar/version/c_970fb48d4fbd8a85
person.familyNameSoares Antunes
person.familyNameSimões
person.familyNameFonseca
person.familyNameFranco
person.familyNameBarroso
person.familyNameGallardo
person.givenNameMónica Sofia
person.givenNameSusana
person.givenNameSuzana
person.givenNameJoão
person.givenNameMário
person.givenNameEugenia
person.identifier.ciencia-idBE1B-DDFA-21F6
person.identifier.ciencia-idC31D-C5F1-D6BD
person.identifier.ciencia-id5110-F476-ECCC
person.identifier.ciencia-idF617-5CA5-EF61
person.identifier.orcid0000-0002-9719-6024
person.identifier.orcid0000-0002-9457-1546
person.identifier.orcid0000-0001-9122-1017
person.identifier.orcid0000-0002-3268-3841
person.identifier.orcid0000-0001-8848-2734
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
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