Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method
Autor(a) principal: | |
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Data de Publicação: | 2008 |
Outros Autores: | |
Tipo de documento: | Artigo |
Idioma: | eng |
Título da fonte: | Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
Texto Completo: | http://hdl.handle.net/10316/5844 https://doi.org/10.1016/j.aca.2007.12.020 |
Resumo: | A Diltiazem kinetic spectrophotometric method was optimized by factorial analysis. The experimental method is based on a two-stage reaction of Diltiazem with hydroxylamine and a ferric salt: in the first stage there is a hydroxamic acid formation; and, in the second stage there is a red colour complex ferric hydroxamate formation. The variables under investigation were: solvent; hydroxylamine, sodium hydroxide and ammonium ferric sulphate concentrations; volume of perchloric acid; and, temperature. The responses of the reactional system were the maximum absorbance, the wavelength and the reaction time at maximum absorbance. Experimental design methodologies were used in the optimization. Fractional and full factorial designs followed by optimization Box-Behnken and central composite experimental designs were used. The observed optimum conditions were: methanol as reaction solvent; hydroxylamine concentration of 9.375%; sodium hydroxide concentration of 18.750%; ferric reagent concentration of 2.000%; minimum volume of perchloric acid to neutralize the sodium hydroxide; and, room temperature as reaction temperature. With this set of experimental conditions a reaction time of 10.5 s with maximum colour development at 512 nm wavelength was achieved. |
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Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification methodAntihypertensor DiltiazemUV-Vis spectroscopyKinetic methodOptimizationExperimental design methodologiesA Diltiazem kinetic spectrophotometric method was optimized by factorial analysis. The experimental method is based on a two-stage reaction of Diltiazem with hydroxylamine and a ferric salt: in the first stage there is a hydroxamic acid formation; and, in the second stage there is a red colour complex ferric hydroxamate formation. The variables under investigation were: solvent; hydroxylamine, sodium hydroxide and ammonium ferric sulphate concentrations; volume of perchloric acid; and, temperature. The responses of the reactional system were the maximum absorbance, the wavelength and the reaction time at maximum absorbance. Experimental design methodologies were used in the optimization. Fractional and full factorial designs followed by optimization Box-Behnken and central composite experimental designs were used. The observed optimum conditions were: methanol as reaction solvent; hydroxylamine concentration of 9.375%; sodium hydroxide concentration of 18.750%; ferric reagent concentration of 2.000%; minimum volume of perchloric acid to neutralize the sodium hydroxide; and, room temperature as reaction temperature. With this set of experimental conditions a reaction time of 10.5 s with maximum colour development at 512 nm wavelength was achieved.http://www.sciencedirect.com/science/article/B6TF4-4RFJ4MK-1/1/520dd87e6a21fc5b354c441c5e92d2072008info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleaplication/PDFhttp://hdl.handle.net/10316/5844http://hdl.handle.net/10316/5844https://doi.org/10.1016/j.aca.2007.12.020engAnalytica Chimica Acta. 609:1 (2008) 1-12Leitão, João M. M.Silva, Joaquim C. G. Esteves dainfo:eu-repo/semantics/openAccessreponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãoinstacron:RCAAP2020-11-06T16:48:44Zoai:estudogeral.uc.pt:10316/5844Portal AgregadorONGhttps://www.rcaap.pt/oai/openaireopendoar:71602024-03-19T20:47:23.596145Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãofalse |
dc.title.none.fl_str_mv |
Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method |
title |
Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method |
spellingShingle |
Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method Leitão, João M. M. Antihypertensor Diltiazem UV-Vis spectroscopy Kinetic method Optimization Experimental design methodologies |
title_short |
Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method |
title_full |
Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method |
title_fullStr |
Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method |
title_full_unstemmed |
Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method |
title_sort |
Factorial analysis optimization of a Diltiazem kinetic spectrophotometric quantification method |
author |
Leitão, João M. M. |
author_facet |
Leitão, João M. M. Silva, Joaquim C. G. Esteves da |
author_role |
author |
author2 |
Silva, Joaquim C. G. Esteves da |
author2_role |
author |
dc.contributor.author.fl_str_mv |
Leitão, João M. M. Silva, Joaquim C. G. Esteves da |
dc.subject.por.fl_str_mv |
Antihypertensor Diltiazem UV-Vis spectroscopy Kinetic method Optimization Experimental design methodologies |
topic |
Antihypertensor Diltiazem UV-Vis spectroscopy Kinetic method Optimization Experimental design methodologies |
description |
A Diltiazem kinetic spectrophotometric method was optimized by factorial analysis. The experimental method is based on a two-stage reaction of Diltiazem with hydroxylamine and a ferric salt: in the first stage there is a hydroxamic acid formation; and, in the second stage there is a red colour complex ferric hydroxamate formation. The variables under investigation were: solvent; hydroxylamine, sodium hydroxide and ammonium ferric sulphate concentrations; volume of perchloric acid; and, temperature. The responses of the reactional system were the maximum absorbance, the wavelength and the reaction time at maximum absorbance. Experimental design methodologies were used in the optimization. Fractional and full factorial designs followed by optimization Box-Behnken and central composite experimental designs were used. The observed optimum conditions were: methanol as reaction solvent; hydroxylamine concentration of 9.375%; sodium hydroxide concentration of 18.750%; ferric reagent concentration of 2.000%; minimum volume of perchloric acid to neutralize the sodium hydroxide; and, room temperature as reaction temperature. With this set of experimental conditions a reaction time of 10.5 s with maximum colour development at 512 nm wavelength was achieved. |
publishDate |
2008 |
dc.date.none.fl_str_mv |
2008 |
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 |
http://hdl.handle.net/10316/5844 http://hdl.handle.net/10316/5844 https://doi.org/10.1016/j.aca.2007.12.020 |
url |
http://hdl.handle.net/10316/5844 https://doi.org/10.1016/j.aca.2007.12.020 |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
Analytica Chimica Acta. 609:1 (2008) 1-12 |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
aplication/PDF |
dc.source.none.fl_str_mv |
reponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação instacron:RCAAP |
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Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação |
instacron_str |
RCAAP |
institution |
RCAAP |
reponame_str |
Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
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Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
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Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação |
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1799133751144349696 |