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: Journal of the Brazilian Chemical Society (Online)
Texto Completo: http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532017000601038
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 injectionLC-MSnLC-SPE-NMRimpurity identificationIdentifying 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 Química2017-06-01info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersiontext/htmlhttp://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532017000601038Journal of the Brazilian Chemical Society v.28 n.6 2017reponame:Journal of the Brazilian Chemical Society (Online)instname:Sociedade Brasileira de Química (SBQ)instacron:SBQ10.21577/0103-5053.20160259info:eu-repo/semantics/openAccessCardoso,Josiane O.Thomasi,Sérgio S.Venâncio,TiagoPitta,Ivan R.Lima,Maria do Carmo A. deOliveira,Regina V.eng2017-05-11T00:00:00Zoai:scielo:S0103-50532017000601038Revistahttp://jbcs.sbq.org.brONGhttps://old.scielo.br/oai/scielo-oai.php||office@jbcs.sbq.org.br1678-47900103-5053opendoar:2017-05-11T00:00Journal of the Brazilian Chemical Society (Online) - Sociedade Brasileira de Química (SBQ)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
LC-MSn
LC-SPE-NMR
impurity identification
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
LC-MSn
LC-SPE-NMR
impurity identification
topic semi-preparative separation
stacked injection
LC-MSn
LC-SPE-NMR
impurity identification
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 2017-06-01
dc.type.driver.fl_str_mv info:eu-repo/semantics/article
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
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status_str publishedVersion
dc.identifier.uri.fl_str_mv http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532017000601038
url http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532017000601038
dc.language.iso.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv 10.21577/0103-5053.20160259
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv text/html
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 v.28 n.6 2017
reponame:Journal of the Brazilian Chemical Society (Online)
instname:Sociedade Brasileira de Química (SBQ)
instacron:SBQ
instname_str Sociedade Brasileira de Química (SBQ)
instacron_str SBQ
institution SBQ
reponame_str Journal of the Brazilian Chemical Society (Online)
collection Journal of the Brazilian Chemical Society (Online)
repository.name.fl_str_mv Journal of the Brazilian Chemical Society (Online) - Sociedade Brasileira de Química (SBQ)
repository.mail.fl_str_mv ||office@jbcs.sbq.org.br
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