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
Autor(a) principal: | |
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Data de Publicação: | 2013 |
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/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. |
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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 |
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1799133708585795584 |