Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples
Autor(a) principal: | |
---|---|
Data de Publicação: | 2017 |
Outros Autores: | , , , , |
Tipo de documento: | Artigo |
Idioma: | eng |
Título da fonte: | Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
Texto Completo: | http://hdl.handle.net/10400.14/23766 |
Resumo: | The accurate assessment of racemic pharmaceuticals requires enantioselective analytical methods. This study presents the development and validation of an enantioselective liquid chromatography with a fluorescence detection method for the concomitant quantification of the enantiomers of tramadol and their metabolites, N-desmethyltramadol and O-desmethyltramadol, in wastewater samples. Optimized conditions were achieved using a Lux Cellulose-4 column 150 × 4.6 mm, 3 μm isocratic elution, and 0.1% diethylamine in hexane and ethanol (96:4, v/v) at 0.7 mL min-1. The samples were extracted using 150 mg Oasis® mixed-mode cation exchange (MCX) cartridges. The method was validated using a synthetic effluent of a laboratory-scale aerobic granular sludge sequencing batch reactor. The method demonstrated to be selective, accurate, and linear (r2 > 0.99) over the range of 56 ng L-1 to 392 ng L-1. The detection and the quantification limits of each enantiomer were 8 ng L-1 and 28 ng L-1 for tramadol and N-desmethyltramadol, and 20 ng L-1 and 56 ng L-1 for O-desmethyltramadol. The feasibility of the method was demonstrated in a screening study in influent and effluent samples from a wastewater treatment plant. The results demonstrated the occurrence of tramadol enantiomers up to 325.1 ng L-1 and 357.9 ng L-1, in the effluent and influent samples, respectively. Both metabolites were detected in influents and effluents. |
id |
RCAP_7b1ab5a453cc3c0b9f272fe105dc8a3c |
---|---|
oai_identifier_str |
oai:repositorio.ucp.pt:10400.14/23766 |
network_acronym_str |
RCAP |
network_name_str |
Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
repository_id_str |
7160 |
spelling |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samplesChiral pharmaceuticalsTramadolN-desmethyltramadolO-desmethyltramadolWastewaterLux Cellulose-4 columnThe accurate assessment of racemic pharmaceuticals requires enantioselective analytical methods. This study presents the development and validation of an enantioselective liquid chromatography with a fluorescence detection method for the concomitant quantification of the enantiomers of tramadol and their metabolites, N-desmethyltramadol and O-desmethyltramadol, in wastewater samples. Optimized conditions were achieved using a Lux Cellulose-4 column 150 × 4.6 mm, 3 μm isocratic elution, and 0.1% diethylamine in hexane and ethanol (96:4, v/v) at 0.7 mL min-1. The samples were extracted using 150 mg Oasis® mixed-mode cation exchange (MCX) cartridges. The method was validated using a synthetic effluent of a laboratory-scale aerobic granular sludge sequencing batch reactor. The method demonstrated to be selective, accurate, and linear (r2 > 0.99) over the range of 56 ng L-1 to 392 ng L-1. The detection and the quantification limits of each enantiomer were 8 ng L-1 and 28 ng L-1 for tramadol and N-desmethyltramadol, and 20 ng L-1 and 56 ng L-1 for O-desmethyltramadol. The feasibility of the method was demonstrated in a screening study in influent and effluent samples from a wastewater treatment plant. The results demonstrated the occurrence of tramadol enantiomers up to 325.1 ng L-1 and 357.9 ng L-1, in the effluent and influent samples, respectively. Both metabolites were detected in influents and effluents.MDPIVeritati - Repositório Institucional da Universidade Católica PortuguesaSilva, CátiaRibeiro, CláudiaMaia, Alexandra S.Gonçalves, VirgíniaTiritan, Maria ElizabethAfonso, Carlos2017-12-19T18:14:05Z20172017-01-01T00:00:00Zinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleapplication/pdfhttp://hdl.handle.net/10400.14/23766engSilva, C., Ribeiro, C., Maia, A. S., Goncalves, V., Tiritan, M. E., & Afonso, C. (2017). Enantiomeric separation of tramadol and its metabolites: Method validation and application to environmental samples. Symmetry-Basel, 9(9), 1702073-899410.3390/sym909017085029418808000411526000003info: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:RCAAP2023-09-12T01:38:23Zoai:repositorio.ucp.pt:10400.14/23766Portal AgregadorONGhttps://www.rcaap.pt/oai/openaireopendoar:71602024-03-19T18:19:30.713376Repositório 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 |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples |
title |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples |
spellingShingle |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples Silva, Cátia Chiral pharmaceuticals Tramadol N-desmethyltramadol O-desmethyltramadol Wastewater Lux Cellulose-4 column |
title_short |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples |
title_full |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples |
title_fullStr |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples |
title_full_unstemmed |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples |
title_sort |
Enantiomeric separation of tramadol and Its metabolites: method validation and application to environmental samples |
author |
Silva, Cátia |
author_facet |
Silva, Cátia Ribeiro, Cláudia Maia, Alexandra S. Gonçalves, Virgínia Tiritan, Maria Elizabeth Afonso, Carlos |
author_role |
author |
author2 |
Ribeiro, Cláudia Maia, Alexandra S. Gonçalves, Virgínia Tiritan, Maria Elizabeth Afonso, Carlos |
author2_role |
author author author author author |
dc.contributor.none.fl_str_mv |
Veritati - Repositório Institucional da Universidade Católica Portuguesa |
dc.contributor.author.fl_str_mv |
Silva, Cátia Ribeiro, Cláudia Maia, Alexandra S. Gonçalves, Virgínia Tiritan, Maria Elizabeth Afonso, Carlos |
dc.subject.por.fl_str_mv |
Chiral pharmaceuticals Tramadol N-desmethyltramadol O-desmethyltramadol Wastewater Lux Cellulose-4 column |
topic |
Chiral pharmaceuticals Tramadol N-desmethyltramadol O-desmethyltramadol Wastewater Lux Cellulose-4 column |
description |
The accurate assessment of racemic pharmaceuticals requires enantioselective analytical methods. This study presents the development and validation of an enantioselective liquid chromatography with a fluorescence detection method for the concomitant quantification of the enantiomers of tramadol and their metabolites, N-desmethyltramadol and O-desmethyltramadol, in wastewater samples. Optimized conditions were achieved using a Lux Cellulose-4 column 150 × 4.6 mm, 3 μm isocratic elution, and 0.1% diethylamine in hexane and ethanol (96:4, v/v) at 0.7 mL min-1. The samples were extracted using 150 mg Oasis® mixed-mode cation exchange (MCX) cartridges. The method was validated using a synthetic effluent of a laboratory-scale aerobic granular sludge sequencing batch reactor. The method demonstrated to be selective, accurate, and linear (r2 > 0.99) over the range of 56 ng L-1 to 392 ng L-1. The detection and the quantification limits of each enantiomer were 8 ng L-1 and 28 ng L-1 for tramadol and N-desmethyltramadol, and 20 ng L-1 and 56 ng L-1 for O-desmethyltramadol. The feasibility of the method was demonstrated in a screening study in influent and effluent samples from a wastewater treatment plant. The results demonstrated the occurrence of tramadol enantiomers up to 325.1 ng L-1 and 357.9 ng L-1, in the effluent and influent samples, respectively. Both metabolites were detected in influents and effluents. |
publishDate |
2017 |
dc.date.none.fl_str_mv |
2017-12-19T18:14:05Z 2017 2017-01-01T00:00:00Z |
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/10400.14/23766 |
url |
http://hdl.handle.net/10400.14/23766 |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
Silva, C., Ribeiro, C., Maia, A. S., Goncalves, V., Tiritan, M. E., & Afonso, C. (2017). Enantiomeric separation of tramadol and its metabolites: Method validation and application to environmental samples. Symmetry-Basel, 9(9), 170 2073-8994 10.3390/sym9090170 85029418808 000411526000003 |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
MDPI |
publisher.none.fl_str_mv |
MDPI |
dc.source.none.fl_str_mv |
reponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação instacron:RCAAP |
instname_str |
Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação |
instacron_str |
RCAAP |
institution |
RCAAP |
reponame_str |
Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
collection |
Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
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 |
repository.mail.fl_str_mv |
|
_version_ |
1799131889824432128 |