Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.

Detalhes bibliográficos
Autor(a) principal: Bergo, Patrícia Luísa de Souza
Data de Publicação: 2009
Outros Autores: Correa, Joane Mariela Miari, Nagem, Tanus Jorge, Augusti, Rodinei, Nascentes, Clésia Cristina
Tipo de documento: Artigo
Idioma: eng
Título da fonte: Repositório Institucional da UFOP
Texto Completo: http://www.repositorio.ufop.br/handle/123456789/5149
http://dx.doi.org/10.1590/S0103-50532009000200021
Resumo: Neste trabalho foi desenvolvido e validado um método quantitativo para a análise de anfetaminas e efedrinas em urina, utilizando-se anidrido acético e piridina, ambos em grau analítico, como derivatizantes. As amostras foram extraídas por extração em fase sólida (EFS), derivatizadas e em seguida analisadas por CG-EM. O método apresentou ampla faixa linear (25-1000 ng mL-1 com R2 > 0,99), alta sensibilidade (LODs variando de 0,0140 a 15,33 ng mL-1 e LOQs variando de 0,0466 a 51,10 ng mL-1), bons índices de precisão (CV < 6% para intra- e inter-ensaios) e excelentes índices de recuperação (87-96%) para todos os compostos estudados. Após a validação, o método foi aplicado em análises de amostras reais de urina humana nas quais ao menos um dos analitos em estudo foi identificado previamente. Em todas as amostras, anfetaminas e efedrinas foram facilmente quantificadas mostrando que a associação de anidrido acético e piridina é uma boa opção como agente derivatizante.
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spelling Bergo, Patrícia Luísa de SouzaCorrea, Joane Mariela MiariNagem, Tanus JorgeAugusti, RodineiNascentes, Clésia Cristina2015-04-24T18:18:23Z2015-04-24T18:18:23Z2009BERGO, P. L. de S. et al. Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents: a suitable approach to reduce costs of routine analyses. Journal of the Brazilian Chemical Society, v. 20, p. 348, 2009. Disponível em: <http://www.scielo.br/scielo.php?pid=s0103-50532009000200021&script=sci_arttext>. Acesso em: 19 fev. 2015.1678-4790http://www.repositorio.ufop.br/handle/123456789/5149http://dx.doi.org/10.1590/S0103-50532009000200021Neste trabalho foi desenvolvido e validado um método quantitativo para a análise de anfetaminas e efedrinas em urina, utilizando-se anidrido acético e piridina, ambos em grau analítico, como derivatizantes. As amostras foram extraídas por extração em fase sólida (EFS), derivatizadas e em seguida analisadas por CG-EM. O método apresentou ampla faixa linear (25-1000 ng mL-1 com R2 > 0,99), alta sensibilidade (LODs variando de 0,0140 a 15,33 ng mL-1 e LOQs variando de 0,0466 a 51,10 ng mL-1), bons índices de precisão (CV < 6% para intra- e inter-ensaios) e excelentes índices de recuperação (87-96%) para todos os compostos estudados. Após a validação, o método foi aplicado em análises de amostras reais de urina humana nas quais ao menos um dos analitos em estudo foi identificado previamente. Em todas as amostras, anfetaminas e efedrinas foram facilmente quantificadas mostrando que a associação de anidrido acético e piridina é uma boa opção como agente derivatizante.A GC/MS method for the simultaneous analyses of different amphetamines and ephedrines in urine employing analytical-grade acetic anhydride/pyridine as derivatizing reagents was developed and validated. Solid-phase extraction was performed on the samples, which were then derivatizated and analyzed by GC/MS. The method showed a broad linear dynamic range (25-1000 ng mL-1 with R2 > 0.99), high sensitivity (LODs of 0.0140 to 15.33 ng mL-1 and LOQs of 0.0466 to 51.10 ng mL-1), good precision (CV < 6% for intra- and inter-assays), and excellent extraction recovery (87 to 96%) for all the compounds studied. After validation, the method was applied in the analyses of real samples of human urine which were previously determined to contain at least one of such drugs. In all the samples, the amphetamines and ephedrines were promptly quantified, showing that the association of acetic anhydride and pyridine can be conveniently employed as a derivatizing agent.StimulantsAmphetaminesEphedrinesUrine analysisDerivatizing reagentsSimultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleO periódico Journal of the Brazilian Chemical Society permite que a UFOP deposite uma cópia em formato eletrônico dos artigos de seus alunos e professores publicados neste periódico no Repositório Institucional. Contato via e-mail em 13 set. 2013.info:eu-repo/semantics/openAccessengreponame:Repositório Institucional da UFOPinstname:Universidade Federal de Ouro Preto (UFOP)instacron:UFOPLICENSElicense.txtlicense.txttext/plain; charset=utf-82636http://www.repositorio.ufop.br/bitstream/123456789/5149/2/license.txtc2ffdd99e58acf69202dff00d361f23aMD52ORIGINALARTIGO_SimultaneousQuantificationAmphetamines.pdfARTIGO_SimultaneousQuantificationAmphetamines.pdfapplication/pdf717287http://www.repositorio.ufop.br/bitstream/123456789/5149/1/ARTIGO_SimultaneousQuantificationAmphetamines.pdf41d1e5adf065673b466c1ee9ebff6fa8MD51123456789/51492019-07-11 12:50:25.602oai:localhost: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Repositório InstitucionalPUBhttp://www.repositorio.ufop.br/oai/requestrepositorio@ufop.edu.bropendoar:32332019-07-11T16:50:25Repositório Institucional da UFOP - Universidade Federal de Ouro Preto (UFOP)false
dc.title.pt_BR.fl_str_mv Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.
title Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.
spellingShingle Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.
Bergo, Patrícia Luísa de Souza
Stimulants
Amphetamines
Ephedrines
Urine analysis
Derivatizing reagents
title_short Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.
title_full Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.
title_fullStr Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.
title_full_unstemmed Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.
title_sort Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents : a suitable approach to reduce costs of routine analyses.
author Bergo, Patrícia Luísa de Souza
author_facet Bergo, Patrícia Luísa de Souza
Correa, Joane Mariela Miari
Nagem, Tanus Jorge
Augusti, Rodinei
Nascentes, Clésia Cristina
author_role author
author2 Correa, Joane Mariela Miari
Nagem, Tanus Jorge
Augusti, Rodinei
Nascentes, Clésia Cristina
author2_role author
author
author
author
dc.contributor.author.fl_str_mv Bergo, Patrícia Luísa de Souza
Correa, Joane Mariela Miari
Nagem, Tanus Jorge
Augusti, Rodinei
Nascentes, Clésia Cristina
dc.subject.por.fl_str_mv Stimulants
Amphetamines
Ephedrines
Urine analysis
Derivatizing reagents
topic Stimulants
Amphetamines
Ephedrines
Urine analysis
Derivatizing reagents
description Neste trabalho foi desenvolvido e validado um método quantitativo para a análise de anfetaminas e efedrinas em urina, utilizando-se anidrido acético e piridina, ambos em grau analítico, como derivatizantes. As amostras foram extraídas por extração em fase sólida (EFS), derivatizadas e em seguida analisadas por CG-EM. O método apresentou ampla faixa linear (25-1000 ng mL-1 com R2 > 0,99), alta sensibilidade (LODs variando de 0,0140 a 15,33 ng mL-1 e LOQs variando de 0,0466 a 51,10 ng mL-1), bons índices de precisão (CV < 6% para intra- e inter-ensaios) e excelentes índices de recuperação (87-96%) para todos os compostos estudados. Após a validação, o método foi aplicado em análises de amostras reais de urina humana nas quais ao menos um dos analitos em estudo foi identificado previamente. Em todas as amostras, anfetaminas e efedrinas foram facilmente quantificadas mostrando que a associação de anidrido acético e piridina é uma boa opção como agente derivatizante.
publishDate 2009
dc.date.issued.fl_str_mv 2009
dc.date.accessioned.fl_str_mv 2015-04-24T18:18:23Z
dc.date.available.fl_str_mv 2015-04-24T18:18:23Z
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dc.type.driver.fl_str_mv info:eu-repo/semantics/article
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dc.identifier.citation.fl_str_mv BERGO, P. L. de S. et al. Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents: a suitable approach to reduce costs of routine analyses. Journal of the Brazilian Chemical Society, v. 20, p. 348, 2009. Disponível em: <http://www.scielo.br/scielo.php?pid=s0103-50532009000200021&script=sci_arttext>. Acesso em: 19 fev. 2015.
dc.identifier.uri.fl_str_mv http://www.repositorio.ufop.br/handle/123456789/5149
dc.identifier.issn.none.fl_str_mv 1678-4790
dc.identifier.doi.none.fl_str_mv http://dx.doi.org/10.1590/S0103-50532009000200021
identifier_str_mv BERGO, P. L. de S. et al. Simultaneous quantification of amphetamines and ephedrines in urine by GC/MS using analytical-grade acetic anhydride/ayridine as derivatizing reagents: a suitable approach to reduce costs of routine analyses. Journal of the Brazilian Chemical Society, v. 20, p. 348, 2009. Disponível em: <http://www.scielo.br/scielo.php?pid=s0103-50532009000200021&script=sci_arttext>. Acesso em: 19 fev. 2015.
1678-4790
url http://www.repositorio.ufop.br/handle/123456789/5149
http://dx.doi.org/10.1590/S0103-50532009000200021
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