Análise de especiação de antimônio em antimoniato de meglumina
Ano de defesa: | 2014 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
Tipo de documento: | Dissertação |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
Brasil
|
Palavras-chave em Português: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/21889 |
Resumo: | In this work the chromatographic conditions for the separation of species of antimony in the drug meglumine antimoniate were optimized. Furthermore, the effect of the treatment with hydrochloric acid in the sample was evaluated in order to convert Sb(III) species and Sb(V) complexed with meglumine in their free inorganic forms. The separation of Sb species was performed by liquid chromatography (LC) in an anion exchange column (PRP-X100) and detection by mass spectrometry with inductively coupled plasma (ICP-MS).The concentrations of Sb obtained by LC-ICP-MS were compared with those obtained by LC-ICP-MS using post-column derivatization by hydride generation (HG). The results of the total concentration of Sb were also evaluated, given by the sum of the concentrations of species determined by LC-ICP-MS, with the results obtained by spectrometry and inductively coupled plasma optical emission (ICP OES). After the evaluations of different mobile phases for separation of Sb species, the selected conditions were: HNO3 15 mmol L -1 at pH 6.0 for 5 min and 20 mmol l -1 EDTA at pH 4.5 for 10 min, both with a flow of 1.0 mL min -1. The presence of at least four kinds of Sb, the two free inorganic (Sb(III) and Sb(V)) and other complexed with meglumine was observed. The results obtained for Sb species in the sample without acid treatment were lower than those obtained for samples with acid treatment. This is probably due to the fact that complexed Sb species have been converted into their free inorganic species of Sb. The result obtained by LC-HG-ICP-MS after sample treatment for Sb(III) species showed no statistical difference (t test, p> 0.05, confidence interval 95%), compared with the result obtained by LC-ICP-MS. Likewise, the result for the total Sb, obtained by ICP OES also no statistically significant difference (t test, p> 0.05, confidence interval 95%) with the addition of Sb species obtained by LC-ICP- MS. Recovery tests were also made, higher concordance found to be 90% and 98% for Sb(V) and Sb(III), respectively. |
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2021-08-11T13:31:51Z2021-08-11T13:31:51Z2014-02-21http://repositorio.ufsm.br/handle/1/21889In this work the chromatographic conditions for the separation of species of antimony in the drug meglumine antimoniate were optimized. Furthermore, the effect of the treatment with hydrochloric acid in the sample was evaluated in order to convert Sb(III) species and Sb(V) complexed with meglumine in their free inorganic forms. The separation of Sb species was performed by liquid chromatography (LC) in an anion exchange column (PRP-X100) and detection by mass spectrometry with inductively coupled plasma (ICP-MS).The concentrations of Sb obtained by LC-ICP-MS were compared with those obtained by LC-ICP-MS using post-column derivatization by hydride generation (HG). The results of the total concentration of Sb were also evaluated, given by the sum of the concentrations of species determined by LC-ICP-MS, with the results obtained by spectrometry and inductively coupled plasma optical emission (ICP OES). After the evaluations of different mobile phases for separation of Sb species, the selected conditions were: HNO3 15 mmol L -1 at pH 6.0 for 5 min and 20 mmol l -1 EDTA at pH 4.5 for 10 min, both with a flow of 1.0 mL min -1. The presence of at least four kinds of Sb, the two free inorganic (Sb(III) and Sb(V)) and other complexed with meglumine was observed. The results obtained for Sb species in the sample without acid treatment were lower than those obtained for samples with acid treatment. This is probably due to the fact that complexed Sb species have been converted into their free inorganic species of Sb. The result obtained by LC-HG-ICP-MS after sample treatment for Sb(III) species showed no statistical difference (t test, p> 0.05, confidence interval 95%), compared with the result obtained by LC-ICP-MS. Likewise, the result for the total Sb, obtained by ICP OES also no statistically significant difference (t test, p> 0.05, confidence interval 95%) with the addition of Sb species obtained by LC-ICP- MS. Recovery tests were also made, higher concordance found to be 90% and 98% for Sb(V) and Sb(III), respectively.Neste trabalho foram otimizadas as condições cromatográficas para a separação de espécies de antimônio no medicamento antimoniato de meglumina. Ademais, foi avaliado o efeito do tratamento da amostra com ácido clorídrico, a fim de converter as espécies Sb(III) e Sb(V), complexadas com a meglumina, em suas formas inorgânicas livres. A separação das espécies de Sb foi feita por cromatografia a líquido (LC) em uma coluna de troca aniônica (PRP-X100) e detecção por espectrometria de massa com plasma indutivamente acoplado (ICP-MS). As concentrações de Sb obtidas por LC-ICP-MS foram comparadas àquelas obtidas por LC-ICP-MS utilizando derivação pós-coluna por geração de hidretos (HG). Também foram comparados os resultados da concentração de Sb total, obtido pelo somatório das concentrações das espécies determinadas por LC-ICP-MS, com os resultados obtidos por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). Após as avaliações de diferentes fases móveis para a separação das espécies de Sb, as condições selecionadas foram: HNO3 15 mmol L-1 em pH 6,0 por 5 min e EDTA 20 mmol L-1 em pH 4,5 por 10 min, ambos com vazão de 1,0 mL min-1. Foi observada a presença de, no mínimo, quatro espécies de Sb, duas na forma inorgânica livre (Sb(III) e Sb(V)) e as outras complexadas com a meglumina. Os resultados obtidos para as espécies de Sb na amostra sem o tratamento ácido foram inferiores aos obtidos para as amostras com tratamento ácido. Isto provavelmente se deve ao fato de as espécies de Sb complexadas terem sido convertidas nas respectivas espécies de Sb inorgânicas livres. O resultado obtido por LC-HG-ICP-MS, após o tratamento da amostra, para a espécie Sb(III) não apresentou diferença estatística (test t, p > 0,05, intervalo de confiança de 95%), comparado ao resultado obtido por LC-ICP-MS. Da mesma forma, o resultado para Sb total, obtido por ICP OES, também não apresentou diferença estatística (test t, p > 0,05, intervalo de confiança de 95%) com o somatório das espécies de Sb obtido por LC-ICP-MS. Também foram feitos ensaios de recuperação sendo encontradas concordâncias superiores a 90% e 98% para Sb(V) e Sb(III), respectivamente.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessAntimônioCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAnálise de especiação de antimônio em antimoniato de megluminainfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisDressler, Valderi Luizhttp://lattes.cnpq.br/4054740296547580Mortari, Sergio RobertoBizzi, Cezar Augustohttp://lattes.cnpq.br/8614644571693365Schons, Franciéli Kaspary10060000000060060060060060029c59cfe-a489-425c-88a5-18fdf7cbf2585da3dcb7-c281-4c06-b42e-03e37d9122d8b4d0ba10-19c4-43bb-8e88-bb2ae6aa3e1bea5d5aeb-956d-4091-b711-982595b3e995reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2014_SCHONS_FRANCIELI.pdfDIS_PPGQUIMICA_2014_SCHONS_FRANCIELI.pdfDissertaçãoapplication/pdf5462618http://repositorio.ufsm.br/bitstream/1/21889/1/DIS_PPGQUIMICA_2014_SCHONS_FRANCIELI.pdf664df2e5d875624e1234fd16bbea0f30MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Análise de especiação de antimônio em antimoniato de meglumina |
title |
Análise de especiação de antimônio em antimoniato de meglumina |
spellingShingle |
Análise de especiação de antimônio em antimoniato de meglumina Schons, Franciéli Kaspary Antimônio CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Análise de especiação de antimônio em antimoniato de meglumina |
title_full |
Análise de especiação de antimônio em antimoniato de meglumina |
title_fullStr |
Análise de especiação de antimônio em antimoniato de meglumina |
title_full_unstemmed |
Análise de especiação de antimônio em antimoniato de meglumina |
title_sort |
Análise de especiação de antimônio em antimoniato de meglumina |
author |
Schons, Franciéli Kaspary |
author_facet |
Schons, Franciéli Kaspary |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Dressler, Valderi Luiz |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4054740296547580 |
dc.contributor.referee1.fl_str_mv |
Mortari, Sergio Roberto |
dc.contributor.referee2.fl_str_mv |
Bizzi, Cezar Augusto |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/8614644571693365 |
dc.contributor.author.fl_str_mv |
Schons, Franciéli Kaspary |
contributor_str_mv |
Dressler, Valderi Luiz Mortari, Sergio Roberto Bizzi, Cezar Augusto |
dc.subject.por.fl_str_mv |
Antimônio |
topic |
Antimônio CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work the chromatographic conditions for the separation of species of antimony in the drug meglumine antimoniate were optimized. Furthermore, the effect of the treatment with hydrochloric acid in the sample was evaluated in order to convert Sb(III) species and Sb(V) complexed with meglumine in their free inorganic forms. The separation of Sb species was performed by liquid chromatography (LC) in an anion exchange column (PRP-X100) and detection by mass spectrometry with inductively coupled plasma (ICP-MS).The concentrations of Sb obtained by LC-ICP-MS were compared with those obtained by LC-ICP-MS using post-column derivatization by hydride generation (HG). The results of the total concentration of Sb were also evaluated, given by the sum of the concentrations of species determined by LC-ICP-MS, with the results obtained by spectrometry and inductively coupled plasma optical emission (ICP OES). After the evaluations of different mobile phases for separation of Sb species, the selected conditions were: HNO3 15 mmol L -1 at pH 6.0 for 5 min and 20 mmol l -1 EDTA at pH 4.5 for 10 min, both with a flow of 1.0 mL min -1. The presence of at least four kinds of Sb, the two free inorganic (Sb(III) and Sb(V)) and other complexed with meglumine was observed. The results obtained for Sb species in the sample without acid treatment were lower than those obtained for samples with acid treatment. This is probably due to the fact that complexed Sb species have been converted into their free inorganic species of Sb. The result obtained by LC-HG-ICP-MS after sample treatment for Sb(III) species showed no statistical difference (t test, p> 0.05, confidence interval 95%), compared with the result obtained by LC-ICP-MS. Likewise, the result for the total Sb, obtained by ICP OES also no statistically significant difference (t test, p> 0.05, confidence interval 95%) with the addition of Sb species obtained by LC-ICP- MS. Recovery tests were also made, higher concordance found to be 90% and 98% for Sb(V) and Sb(III), respectively. |
publishDate |
2014 |
dc.date.issued.fl_str_mv |
2014-02-21 |
dc.date.accessioned.fl_str_mv |
2021-08-11T13:31:51Z |
dc.date.available.fl_str_mv |
2021-08-11T13:31:51Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/21889 |
url |
http://repositorio.ufsm.br/handle/1/21889 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 |
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dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
eu_rights_str_mv |
openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
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