A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry

Detalhes bibliográficos
Autor(a) principal: Margalho, Cláudia
Data de Publicação: 2013
Outros Autores: Gallardo, Eugenia, Castanheira, Alice, Vieira, Duarte Nuno, López-Rivadulla, Manuel, Real, Francisco Corte
Tipo de documento: Artigo
Idioma: eng
Título da fonte: Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
Texto Completo: http://hdl.handle.net/10316/27255
https://doi.org/10.1016/j.chroma.2013.07.031
Resumo: The use of vitreous humor and pericardial fluid as alternative matrices to blood and plasma in the field of forensic toxicology is described to quantitate low levels of Salvinorin A using ethion as internal standard. The method was optimized and fully validated using international accepted guidelines. The developed methodology utilizes a solid phase extraction procedure coupled to gas chromatography mass spectrometry operated in the selected ion monitoring mode. The method was linear in the range of 5.0–100 ng/mL with determination coefficients higher than 0.99 in 100 μL of vitreous humor and in 250 μL of each matrix pericardial fluid, whole blood and plasma. The limits of detection and quantitation were experimentally determined as 5.0 ng/mL, intra-day precision, intermediate precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The sample cleanup step presented mean efficiencies between 80 and 106% in the different biological specimens analyzed. According to the low volumes of samples used, and the low limits achieved using a single quadrupole mass spectrometer, which is available in most laboratories, we can conclude that the validated methodology is sensitive and simple and is suitable for the application in forensic toxicology laboratories for the routine analysis of Salvinorin A in both conventional and unconventional biological samples.
id RCAP_97e7f132f1aac607ad288d2c942c2b0e
oai_identifier_str oai:estudogeral.uc.pt:10316/27255
network_acronym_str RCAP
network_name_str Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
repository_id_str 7160
spelling A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometrySalvinorin ABiological specimensSPEGC-MS-EIThe use of vitreous humor and pericardial fluid as alternative matrices to blood and plasma in the field of forensic toxicology is described to quantitate low levels of Salvinorin A using ethion as internal standard. The method was optimized and fully validated using international accepted guidelines. The developed methodology utilizes a solid phase extraction procedure coupled to gas chromatography mass spectrometry operated in the selected ion monitoring mode. The method was linear in the range of 5.0–100 ng/mL with determination coefficients higher than 0.99 in 100 μL of vitreous humor and in 250 μL of each matrix pericardial fluid, whole blood and plasma. The limits of detection and quantitation were experimentally determined as 5.0 ng/mL, intra-day precision, intermediate precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The sample cleanup step presented mean efficiencies between 80 and 106% in the different biological specimens analyzed. According to the low volumes of samples used, and the low limits achieved using a single quadrupole mass spectrometer, which is available in most laboratories, we can conclude that the validated methodology is sensitive and simple and is suitable for the application in forensic toxicology laboratories for the routine analysis of Salvinorin A in both conventional and unconventional biological samples.Elsevier2013-08-23info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articlehttp://hdl.handle.net/10316/27255http://hdl.handle.net/10316/27255https://doi.org/10.1016/j.chroma.2013.07.031engMARGALHO, Claúdia [et. al] - A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry. "Journal of Chromatography A". ISSN 0021-9673. Vol. 1304 (2013) p. 203-2100021-9673http://www.sciencedirect.com/science/article/pii/S0021967313010753Margalho, CláudiaGallardo, EugeniaCastanheira, AliceVieira, Duarte NunoLópez-Rivadulla, ManuelReal, Francisco Corteinfo: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:RCAAP2022-05-25T06:46:58Zoai:estudogeral.uc.pt:10316/27255Portal AgregadorONGhttps://www.rcaap.pt/oai/openaireopendoar:71602024-03-19T20:43:40.429686Repositório 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 A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry
title A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry
spellingShingle A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry
Margalho, Cláudia
Salvinorin A
Biological specimens
SPE
GC-MS-EI
title_short A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry
title_full A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry
title_fullStr A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry
title_full_unstemmed A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry
title_sort A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry
author Margalho, Cláudia
author_facet Margalho, Cláudia
Gallardo, Eugenia
Castanheira, Alice
Vieira, Duarte Nuno
López-Rivadulla, Manuel
Real, Francisco Corte
author_role author
author2 Gallardo, Eugenia
Castanheira, Alice
Vieira, Duarte Nuno
López-Rivadulla, Manuel
Real, Francisco Corte
author2_role author
author
author
author
author
dc.contributor.author.fl_str_mv Margalho, Cláudia
Gallardo, Eugenia
Castanheira, Alice
Vieira, Duarte Nuno
López-Rivadulla, Manuel
Real, Francisco Corte
dc.subject.por.fl_str_mv Salvinorin A
Biological specimens
SPE
GC-MS-EI
topic Salvinorin A
Biological specimens
SPE
GC-MS-EI
description The use of vitreous humor and pericardial fluid as alternative matrices to blood and plasma in the field of forensic toxicology is described to quantitate low levels of Salvinorin A using ethion as internal standard. The method was optimized and fully validated using international accepted guidelines. The developed methodology utilizes a solid phase extraction procedure coupled to gas chromatography mass spectrometry operated in the selected ion monitoring mode. The method was linear in the range of 5.0–100 ng/mL with determination coefficients higher than 0.99 in 100 μL of vitreous humor and in 250 μL of each matrix pericardial fluid, whole blood and plasma. The limits of detection and quantitation were experimentally determined as 5.0 ng/mL, intra-day precision, intermediate precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The sample cleanup step presented mean efficiencies between 80 and 106% in the different biological specimens analyzed. According to the low volumes of samples used, and the low limits achieved using a single quadrupole mass spectrometer, which is available in most laboratories, we can conclude that the validated methodology is sensitive and simple and is suitable for the application in forensic toxicology laboratories for the routine analysis of Salvinorin A in both conventional and unconventional biological samples.
publishDate 2013
dc.date.none.fl_str_mv 2013-08-23
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/10316/27255
http://hdl.handle.net/10316/27255
https://doi.org/10.1016/j.chroma.2013.07.031
url http://hdl.handle.net/10316/27255
https://doi.org/10.1016/j.chroma.2013.07.031
dc.language.iso.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv MARGALHO, Claúdia [et. al] - A validated procedure for detection and quantitation of salvinorin a in pericardial fluid, vitreous humor, whole blood and plasma using solid phase extraction and gas chromatography–mass spectrometry. "Journal of Chromatography A". ISSN 0021-9673. Vol. 1304 (2013) p. 203-210
0021-9673
http://www.sciencedirect.com/science/article/pii/S0021967313010753
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
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_ 1799133708585795584