Preparative Separation and Structural Identification of Impurities of a New α2-Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR
Autor(a) principal: | |
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Data de Publicação: | 2017 |
Outros Autores: | , , , , |
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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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 |
format |
article |
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 |
_version_ |
1750318179568058368 |