Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR

Detalhes bibliográficos
Autor(a) principal: Cardoso, Josiane O.
Data de Publicação: 2017
Outros Autores: Thomasi, Sérgio S., Venâncio, Tiago, Pitta, Ivan R., Lima, Maria do Carmo A. de, Oliveira, Regina V.
Tipo de documento: Artigo
Idioma: eng
Título da fonte: Repositório Institucional da UFLA
Texto Completo: http://repositorio.ufla.br/jspui/handle/1/32516
Resumo: Identifying impurities in drug substances has become one of the most important issues in pharmaceutical analysis since it can have a significant impact on the efficacy of new pharmaceutical products. Due to the purity requirements, in this paper a new synthetic α2-adrenoceptor agonist, called LPSF-PT-31, was purified and its impurities were characterized by liquid chromatography-multistage mass spectrometry (LC-MSn) and liquid chromatography-solid phase extraction-nuclear magnetic resonance (LC-SPE-NMR). The purification step was conducted using a semi-preparative liquid chromatography and stacked injections as a new approach to drug purification. As a result, a total yield of 75% of the pure LPSF-PT-31 and 2.9 L day-1 in solvent reduction was obtained. The combination of semi-preparative stacking injection, LC-MSn, and LC-SPE-NMR, demonstrated to be efficient to purify active drugs and unambiguously identify its impurities. In addition, isolation and identification of drug impurities in the early stages of development can improve the synthetic pathway, preventing the formation of impurities or minimizing this formation to minimum levels.
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spelling Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMRSemi-preparative separationStacked injectionImpurity identificationSeparação semi-preparativaInjeção empilhadaIdentificação de impurezasIdentifying impurities in drug substances has become one of the most important issues in pharmaceutical analysis since it can have a significant impact on the efficacy of new pharmaceutical products. Due to the purity requirements, in this paper a new synthetic α2-adrenoceptor agonist, called LPSF-PT-31, was purified and its impurities were characterized by liquid chromatography-multistage mass spectrometry (LC-MSn) and liquid chromatography-solid phase extraction-nuclear magnetic resonance (LC-SPE-NMR). The purification step was conducted using a semi-preparative liquid chromatography and stacked injections as a new approach to drug purification. As a result, a total yield of 75% of the pure LPSF-PT-31 and 2.9 L day-1 in solvent reduction was obtained. The combination of semi-preparative stacking injection, LC-MSn, and LC-SPE-NMR, demonstrated to be efficient to purify active drugs and unambiguously identify its impurities. In addition, isolation and identification of drug impurities in the early stages of development can improve the synthetic pathway, preventing the formation of impurities or minimizing this formation to minimum levels.Sociedade Brasileira de Química2019-01-25T09:52:26Z2019-01-25T09:52:26Z2017-06info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleapplication/pdfCARDOSO, J. O. et al. Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR. Journal of the Brazilian Chemical Society, São Paulo, v. 28, n. 6, p. 1038-1047, June 2017.http://repositorio.ufla.br/jspui/handle/1/32516Journal of the Brazilian Chemical Societyreponame:Repositório Institucional da UFLAinstname:Universidade Federal de Lavras (UFLA)instacron:UFLAhttp://creativecommons.org/licenses/by/4.0/info:eu-repo/semantics/openAccessCardoso, Josiane O.Thomasi, Sérgio S.Venâncio, TiagoPitta, Ivan R.Lima, Maria do Carmo A. deOliveira, Regina V.eng2019-01-25T09:52:26Zoai:localhost:1/32516Repositório InstitucionalPUBhttp://repositorio.ufla.br/oai/requestnivaldo@ufla.br || repositorio.biblioteca@ufla.bropendoar:2019-01-25T09:52:26Repositório Institucional da UFLA - Universidade Federal de Lavras (UFLA)false
dc.title.none.fl_str_mv Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
title Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
spellingShingle Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
Cardoso, Josiane O.
Semi-preparative separation
Stacked injection
Impurity identification
Separação semi-preparativa
Injeção empilhada
Identificação de impurezas
title_short Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
title_full Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
title_fullStr Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
title_full_unstemmed Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
title_sort Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
author Cardoso, Josiane O.
author_facet Cardoso, Josiane O.
Thomasi, Sérgio S.
Venâncio, Tiago
Pitta, Ivan R.
Lima, Maria do Carmo A. de
Oliveira, Regina V.
author_role author
author2 Thomasi, Sérgio S.
Venâncio, Tiago
Pitta, Ivan R.
Lima, Maria do Carmo A. de
Oliveira, Regina V.
author2_role author
author
author
author
author
dc.contributor.author.fl_str_mv Cardoso, Josiane O.
Thomasi, Sérgio S.
Venâncio, Tiago
Pitta, Ivan R.
Lima, Maria do Carmo A. de
Oliveira, Regina V.
dc.subject.por.fl_str_mv Semi-preparative separation
Stacked injection
Impurity identification
Separação semi-preparativa
Injeção empilhada
Identificação de impurezas
topic Semi-preparative separation
Stacked injection
Impurity identification
Separação semi-preparativa
Injeção empilhada
Identificação de impurezas
description Identifying impurities in drug substances has become one of the most important issues in pharmaceutical analysis since it can have a significant impact on the efficacy of new pharmaceutical products. Due to the purity requirements, in this paper a new synthetic α2-adrenoceptor agonist, called LPSF-PT-31, was purified and its impurities were characterized by liquid chromatography-multistage mass spectrometry (LC-MSn) and liquid chromatography-solid phase extraction-nuclear magnetic resonance (LC-SPE-NMR). The purification step was conducted using a semi-preparative liquid chromatography and stacked injections as a new approach to drug purification. As a result, a total yield of 75% of the pure LPSF-PT-31 and 2.9 L day-1 in solvent reduction was obtained. The combination of semi-preparative stacking injection, LC-MSn, and LC-SPE-NMR, demonstrated to be efficient to purify active drugs and unambiguously identify its impurities. In addition, isolation and identification of drug impurities in the early stages of development can improve the synthetic pathway, preventing the formation of impurities or minimizing this formation to minimum levels.
publishDate 2017
dc.date.none.fl_str_mv 2017-06
2019-01-25T09:52:26Z
2019-01-25T09:52:26Z
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 CARDOSO, J. O. et al. Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR. Journal of the Brazilian Chemical Society, São Paulo, v. 28, n. 6, p. 1038-1047, June 2017.
http://repositorio.ufla.br/jspui/handle/1/32516
identifier_str_mv CARDOSO, J. O. et al. Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR. Journal of the Brazilian Chemical Society, São Paulo, v. 28, n. 6, p. 1038-1047, June 2017.
url http://repositorio.ufla.br/jspui/handle/1/32516
dc.language.iso.fl_str_mv eng
language eng
dc.rights.driver.fl_str_mv http://creativecommons.org/licenses/by/4.0/
info:eu-repo/semantics/openAccess
rights_invalid_str_mv http://creativecommons.org/licenses/by/4.0/
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Sociedade Brasileira de Química
publisher.none.fl_str_mv Sociedade Brasileira de Química
dc.source.none.fl_str_mv Journal of the Brazilian Chemical Society
reponame:Repositório Institucional da UFLA
instname:Universidade Federal de Lavras (UFLA)
instacron:UFLA
instname_str Universidade Federal de Lavras (UFLA)
instacron_str UFLA
institution UFLA
reponame_str Repositório Institucional da UFLA
collection Repositório Institucional da UFLA
repository.name.fl_str_mv Repositório Institucional da UFLA - Universidade Federal de Lavras (UFLA)
repository.mail.fl_str_mv nivaldo@ufla.br || repositorio.biblioteca@ufla.br
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