Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography
Autor(a) principal: | |
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Data de Publicação: | 2015 |
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=S0103-50532015000500887 |
Resumo: | A methodology for the simultaneous determination of nelfinavir mesylate and the impurities 3-hydroxy-2-methylbenzoic acid and (2R,3R)-4-((3S,4aS,8aS)-3-(tert-butylcarbamoyl) octahydroisoquinolin-2(1H)-yl)-3-hydroxy-1-(phenylthio)butan-2-aminium benzoate by micellar electrokinetic chromatography, with an analysis time of 25 min, was proposed. An electrolyte composed of sodium tetraborate buffer (pH 9.24; 25 mmol L-1), sodium dodecyl sulphate (9 mmol L-1) and methanol (10%, v/v) was optimized using a mixed-level factorial design, with direct detection at 200 nm. After evaluating some figures of merit, such as selectivity, linearity, precision, limit of detection, limit of quantification, accuracy and robustness (using Youden's test), the method was successfully applied to the analysis of nelfinavir mesylate and its impurities in a pharmaceutical formulation. The optimized methodology is demonstrated to be useful in the determination of these analytes in a synthesis monitoring process, in raw materials and in pharmaceutical formulations, while offering low solvent consumption, requiring a small sample and using non-specific columns as advantages. |
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Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatographynelfinavirimpuritiesmicellar electrokinetic chromatographymixed factorial designYouden's testA methodology for the simultaneous determination of nelfinavir mesylate and the impurities 3-hydroxy-2-methylbenzoic acid and (2R,3R)-4-((3S,4aS,8aS)-3-(tert-butylcarbamoyl) octahydroisoquinolin-2(1H)-yl)-3-hydroxy-1-(phenylthio)butan-2-aminium benzoate by micellar electrokinetic chromatography, with an analysis time of 25 min, was proposed. An electrolyte composed of sodium tetraborate buffer (pH 9.24; 25 mmol L-1), sodium dodecyl sulphate (9 mmol L-1) and methanol (10%, v/v) was optimized using a mixed-level factorial design, with direct detection at 200 nm. After evaluating some figures of merit, such as selectivity, linearity, precision, limit of detection, limit of quantification, accuracy and robustness (using Youden's test), the method was successfully applied to the analysis of nelfinavir mesylate and its impurities in a pharmaceutical formulation. The optimized methodology is demonstrated to be useful in the determination of these analytes in a synthesis monitoring process, in raw materials and in pharmaceutical formulations, while offering low solvent consumption, requiring a small sample and using non-specific columns as advantages.Sociedade Brasileira de Química2015-05-01info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersiontext/htmlhttp://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532015000500887Journal of the Brazilian Chemical Society v.26 n.5 2015reponame:Journal of the Brazilian Chemical Society (Online)instname:Sociedade Brasileira de Química (SBQ)instacron:SBQ10.5935/0103-5053.20150049info:eu-repo/semantics/openAccessBastos,Carina A.Gomes,Cláudia R. B.Souza,Marcus V. N. deOliveira,Marcone A. L. deeng2015-10-26T00:00:00Zoai:scielo:S0103-50532015000500887Revistahttp://jbcs.sbq.org.brONGhttps://old.scielo.br/oai/scielo-oai.php||office@jbcs.sbq.org.br1678-47900103-5053opendoar:2015-10-26T00:00Journal of the Brazilian Chemical Society (Online) - Sociedade Brasileira de Química (SBQ)false |
dc.title.none.fl_str_mv |
Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography |
title |
Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography |
spellingShingle |
Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography Bastos,Carina A. nelfinavir impurities micellar electrokinetic chromatography mixed factorial design Youden's test |
title_short |
Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography |
title_full |
Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography |
title_fullStr |
Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography |
title_full_unstemmed |
Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography |
title_sort |
Optimization of an Electrolyte System for the Simultaneous Separation of Nelfinavir Mesylate and Two Impurities by Micellar Electrokinetic Chromatography |
author |
Bastos,Carina A. |
author_facet |
Bastos,Carina A. Gomes,Cláudia R. B. Souza,Marcus V. N. de Oliveira,Marcone A. L. de |
author_role |
author |
author2 |
Gomes,Cláudia R. B. Souza,Marcus V. N. de Oliveira,Marcone A. L. de |
author2_role |
author author author |
dc.contributor.author.fl_str_mv |
Bastos,Carina A. Gomes,Cláudia R. B. Souza,Marcus V. N. de Oliveira,Marcone A. L. de |
dc.subject.por.fl_str_mv |
nelfinavir impurities micellar electrokinetic chromatography mixed factorial design Youden's test |
topic |
nelfinavir impurities micellar electrokinetic chromatography mixed factorial design Youden's test |
description |
A methodology for the simultaneous determination of nelfinavir mesylate and the impurities 3-hydroxy-2-methylbenzoic acid and (2R,3R)-4-((3S,4aS,8aS)-3-(tert-butylcarbamoyl) octahydroisoquinolin-2(1H)-yl)-3-hydroxy-1-(phenylthio)butan-2-aminium benzoate by micellar electrokinetic chromatography, with an analysis time of 25 min, was proposed. An electrolyte composed of sodium tetraborate buffer (pH 9.24; 25 mmol L-1), sodium dodecyl sulphate (9 mmol L-1) and methanol (10%, v/v) was optimized using a mixed-level factorial design, with direct detection at 200 nm. After evaluating some figures of merit, such as selectivity, linearity, precision, limit of detection, limit of quantification, accuracy and robustness (using Youden's test), the method was successfully applied to the analysis of nelfinavir mesylate and its impurities in a pharmaceutical formulation. The optimized methodology is demonstrated to be useful in the determination of these analytes in a synthesis monitoring process, in raw materials and in pharmaceutical formulations, while offering low solvent consumption, requiring a small sample and using non-specific columns as advantages. |
publishDate |
2015 |
dc.date.none.fl_str_mv |
2015-05-01 |
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=S0103-50532015000500887 |
url |
http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532015000500887 |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
10.5935/0103-5053.20150049 |
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.26 n.5 2015 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_ |
1750318177065107456 |