Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood

Detalhes bibliográficos
Autor(a) principal: Júlio, Sara
Data de Publicação: 2023
Outros Autores: Ferro, Raquel A., Santos, Susana, Alexandre, Andrea, Caldeira, Maria João, Franco, João, Barroso, Mário, Gaspar, Helena
Tipo de documento: Artigo
Idioma: eng
Título da fonte: Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
Texto Completo: http://hdl.handle.net/10400.8/8733
Resumo: This work was supported by the Portuguese Foundation for Science and Technology (FCT) through Strategic Projects UIDP/04046/2020 and UIDB/04046/2020 to BioISI—BioSystems and Integrative Sciences Institute; UID/04292/2020 to MARE—Marine and Environmental Sciences Centre; CQE—UIDB/00100/2020, UIDP/00100/2020, and IMS—LA/P/0056/2020, to Centro de Química Estrutural, Institute of Molecular Sciences; Portuguese Mass Spectrometry Network (LISBOA-01-0145FEDER-022125) and National NMR Network (PTNMR), partially supported by Infrastructure Project N° 022161 (co-financed by FEDER through COMPETE 2020, POCI and PORL and FCT through PIDDAC).
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spelling Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in bloodNPSSynthetic cathinonesNMRBloodGC–MSThis work was supported by the Portuguese Foundation for Science and Technology (FCT) through Strategic Projects UIDP/04046/2020 and UIDB/04046/2020 to BioISI—BioSystems and Integrative Sciences Institute; UID/04292/2020 to MARE—Marine and Environmental Sciences Centre; CQE—UIDB/00100/2020, UIDP/00100/2020, and IMS—LA/P/0056/2020, to Centro de Química Estrutural, Institute of Molecular Sciences; Portuguese Mass Spectrometry Network (LISBOA-01-0145FEDER-022125) and National NMR Network (PTNMR), partially supported by Infrastructure Project N° 022161 (co-financed by FEDER through COMPETE 2020, POCI and PORL and FCT through PIDDAC).Over the past 15 years, synthetic cathinones have emerged as an important class of new psychoactive substances (NPS) worldwide. The proliferation of these psychostimulants and their sought-after effects among recreational drug users pose a serious threat to public health and enormous challenges to forensic laboratories. For forensic institutions, it is essential to be one step ahead of covert laboratories, foreseeing the structural changes possible to introduce in the core skeleton of cathinones while maintaining their stimulating activity. In this manner, it is feasible to equip themselves with standards of possible new cathinones and validated analytical methods for their qualitative and quantitative detection. Therefore, the aim of the work herein described was to synthesize emerging cathinones based on the evolving patterns in the illicit drug market, and to develop an analytical method for their accurate determination in forensic situations. Five so far unreported cathinones [4′-methyl-N-dimethylbuphedrone (4-MDMB), 4′-methyl-N-ethylbuphedrone (4-MNEB), 4′-methyl-N-dimethylpentedrone (4-MDMP), 4′-methyl-N-dimethylhexedrone (4-MDMH), and 4′-methyl-N-diethylbuphedrone (4-MDEB)] and a sixth one, 4′-methyl-N-ethylpentedrone, already reported to EMCDDA and also known as 4-MEAP, were synthesized and fully characterized by nuclear magnetic resonance (NMR) spectroscopy and mass spectrometry (MS). An analytical method for the simultaneous quantification of these cathinones in blood, using solid phase extraction (SPE) combined with gas chromatography-mass spectrometry (GC–MS) was developed and validated. The results prove that this methodology is selective, linear, precise, and accurate. For all target cathinones, the extraction efficiency was higher than 73%, linearity was observed in the range of 10 (lower limit of quantification, LLOQ) to 800 ng/mL, with coefficients of determination higher than 0.99, and the limits of detection (LODs) were 5 ng/mL for all target cathinones. The stability of these cathinones in blood matrices is dependent on the storage conditions; 4-MNEB is the most stable compound and 4-MDMH is the least stable compound. The low limits obtained allow the detection of the compounds in situations where they are involved, even if present at low concentrations.SpringerIC-OnlineJúlio, SaraFerro, Raquel A.Santos, SusanaAlexandre, AndreaCaldeira, Maria JoãoFranco, JoãoBarroso, MárioGaspar, Helena2023-08-24T11:20:55Z20232023-01-01T00:00:00Zinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleapplication/pdfhttp://hdl.handle.net/10400.8/8733engJúlio S, Ferro RA, Santos S, Alexandre A, Caldeira MJ, Franco J, Barroso M, Gaspar H. Synthesis of emerging cathinones and validation of a SPE GC-MS method for their simultaneous quantification in blood. Anal Bioanal Chem. 2023 Feb;415(4):571-589. doi: 10.1007/s00216-022-04440-6. Epub 2022 Dec 9. PMID: 36494605.1618-264210.1007/s00216-022-04440-6metadata only accessinfo:eu-repo/semantics/openAccessreponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãoinstacron:RCAAP2024-01-17T15:58:04Zoai:iconline.ipleiria.pt:10400.8/8733Portal AgregadorONGhttps://www.rcaap.pt/oai/openaireopendoar:71602024-03-20T01:51:23.833462Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãofalse
dc.title.none.fl_str_mv Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood
title Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood
spellingShingle Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood
Júlio, Sara
NPS
Synthetic cathinones
NMR
Blood
GC–MS
title_short Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood
title_full Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood
title_fullStr Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood
title_full_unstemmed Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood
title_sort Synthesis of emerging cathinones and validation of a SPE GC–MS method for their simultaneous quantification in blood
author Júlio, Sara
author_facet Júlio, Sara
Ferro, Raquel A.
Santos, Susana
Alexandre, Andrea
Caldeira, Maria João
Franco, João
Barroso, Mário
Gaspar, Helena
author_role author
author2 Ferro, Raquel A.
Santos, Susana
Alexandre, Andrea
Caldeira, Maria João
Franco, João
Barroso, Mário
Gaspar, Helena
author2_role author
author
author
author
author
author
author
dc.contributor.none.fl_str_mv IC-Online
dc.contributor.author.fl_str_mv Júlio, Sara
Ferro, Raquel A.
Santos, Susana
Alexandre, Andrea
Caldeira, Maria João
Franco, João
Barroso, Mário
Gaspar, Helena
dc.subject.por.fl_str_mv NPS
Synthetic cathinones
NMR
Blood
GC–MS
topic NPS
Synthetic cathinones
NMR
Blood
GC–MS
description This work was supported by the Portuguese Foundation for Science and Technology (FCT) through Strategic Projects UIDP/04046/2020 and UIDB/04046/2020 to BioISI—BioSystems and Integrative Sciences Institute; UID/04292/2020 to MARE—Marine and Environmental Sciences Centre; CQE—UIDB/00100/2020, UIDP/00100/2020, and IMS—LA/P/0056/2020, to Centro de Química Estrutural, Institute of Molecular Sciences; Portuguese Mass Spectrometry Network (LISBOA-01-0145FEDER-022125) and National NMR Network (PTNMR), partially supported by Infrastructure Project N° 022161 (co-financed by FEDER through COMPETE 2020, POCI and PORL and FCT through PIDDAC).
publishDate 2023
dc.date.none.fl_str_mv 2023-08-24T11:20:55Z
2023
2023-01-01T00:00:00Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/article
format article
status_str publishedVersion
dc.identifier.uri.fl_str_mv http://hdl.handle.net/10400.8/8733
url http://hdl.handle.net/10400.8/8733
dc.language.iso.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv Júlio S, Ferro RA, Santos S, Alexandre A, Caldeira MJ, Franco J, Barroso M, Gaspar H. Synthesis of emerging cathinones and validation of a SPE GC-MS method for their simultaneous quantification in blood. Anal Bioanal Chem. 2023 Feb;415(4):571-589. doi: 10.1007/s00216-022-04440-6. Epub 2022 Dec 9. PMID: 36494605.
1618-2642
10.1007/s00216-022-04440-6
dc.rights.driver.fl_str_mv metadata only access
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rights_invalid_str_mv metadata only access
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Springer
publisher.none.fl_str_mv Springer
dc.source.none.fl_str_mv reponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
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instacron:RCAAP
instname_str Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação
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repository.name.fl_str_mv Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação
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