Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico
Ano de defesa: | 2014 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
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/1/11988 |
Resumo: | In this work, sample preparation methods were proposed, microwave-induced combustion (MIC) and microwave-assisted wet digestion (MAWD), for further Br, Cl, Cr, Cu, I and Mn determination in pharmaceutical capsules. For Cl, Br and I determination, ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) were used. The ICP-MS technique was also used for Cr, Cu and Mn determination, as well as graphite furnace atomic absorption spectrometry (GF AAS) and by solid sampling graphite furnace atomic absorption spectrometry (SS GF AAS). For MAWD digestion, it was possible to digest 300 mg samples, whereas in MIC up to 500 mg of sample were used. Also, MIC digestion allowed the digestion using diluted nitric acid for all elements, except for Br and I which require diluted alkaline solution. The carbon content was determined in samples after decomposition in order to evaluate the efficiency of decomposition. Sample decomposition was complete for all sample preparation methods applied, since the carbon content in MAWD solutions was 60 mg L-1 and it was lower than the limit of detection (10 mg L-1) for MIC solutions. Certified reference material of whole milk powder was used to evaluate the accuracy of MIC digestion and the agreement to certified values was between 94 and 102%. In conclusion, the investigated sample preparation methods were suitable to pharmaceutical capsules digestion as well as for the determination techniques. Also, chlorine recovery was possible with diluted acid solutions in MIC digestion. |
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2017-11-08T12:35:23Z2017-11-08T12:35:23Z2014http://repositorio.ufsm.br/handle/1/11988In this work, sample preparation methods were proposed, microwave-induced combustion (MIC) and microwave-assisted wet digestion (MAWD), for further Br, Cl, Cr, Cu, I and Mn determination in pharmaceutical capsules. For Cl, Br and I determination, ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) were used. The ICP-MS technique was also used for Cr, Cu and Mn determination, as well as graphite furnace atomic absorption spectrometry (GF AAS) and by solid sampling graphite furnace atomic absorption spectrometry (SS GF AAS). For MAWD digestion, it was possible to digest 300 mg samples, whereas in MIC up to 500 mg of sample were used. Also, MIC digestion allowed the digestion using diluted nitric acid for all elements, except for Br and I which require diluted alkaline solution. The carbon content was determined in samples after decomposition in order to evaluate the efficiency of decomposition. Sample decomposition was complete for all sample preparation methods applied, since the carbon content in MAWD solutions was 60 mg L-1 and it was lower than the limit of detection (10 mg L-1) for MIC solutions. Certified reference material of whole milk powder was used to evaluate the accuracy of MIC digestion and the agreement to certified values was between 94 and 102%. In conclusion, the investigated sample preparation methods were suitable to pharmaceutical capsules digestion as well as for the determination techniques. Also, chlorine recovery was possible with diluted acid solutions in MIC digestion.Neste trabalho foram avaliados dois métodos de preparo de amostra, combustão iniciada por micro-ondas (MIC) e decomposição via úmida assistida por radiação micro-ondas (MAWD), para a posterior determinação de Br, Cl, Cr, Cu, I e Mn em cápsulas de uso farmacêutico. A determinação de Cl, Br e I foi feita por espectrometria de massa com plasma indutivamente acoplado (ICP-MS) e por cromatografia de íons (IC). Por outro lado, a determinação de Cr, Cu e Mn foi feita por ICP-MS, por espectrometria de absorção atômica com forno de grafite (GF AAS) e por análise por amostragem direta de sólidos acoplada a GF AAS (SS GF AAS). A decomposição por MAWD possibilitou o uso de 300 mg de amostra, enquanto que, para MIC, foi possível decompor até 500 mg de amostra. Foi possível a utilização de HNO3 diluído para a absorção dos analitos, exceto para Br e I onde foi necessário o uso de soluções alcalinas diluídas. Para a determinação de Cl foi possível a utilização de HNO3 diluído como solução absorvedora durante a MIC, assim como soluções alcalinas diluídas. A eficiência dos métodos de decomposição foi avaliada através da determinação de carbono residual nas soluções obtidas após MIC e MAWD. Foi observado que o valor de carbono residual nas soluções obtidas após MAWD foi de, aproximadamente, 60 mg L-1 e, nas soluções após MIC, foi inferior ao limite de detecção (10 mg L-1), o que demonstra a boa eficiência de decomposição das amostras por ambos os métodos utilizados. A exatidão do método empregando MIC foi avaliada através da análise de material de referência certificado (CRM) de leite em pó. As concordâncias obtidas para todos os elementos foram entre 94 e 102%. Pode-se concluir que os métodos de preparo de amostra avaliados foram adequados à decomposição das amostras, assim como às técnicas utilizadas para a determinação dos analitos. Cabe destacar, também, que foi possível a recuperação de Cl nas amostras e no CRM utilizando ácido diluído como solução absorvedora durante as decomposições por MIC.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/openAccessQuímica analíticaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAvaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêuticoinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Costa, Adilson Ben dahttp://lattes.cnpq.br/2604778196819181Mello, Paola de Azevedohttp://lattes.cnpq.br/2189500441942469Dressler, Valderi Luizhttp://lattes.cnpq.br/4054740296547580Mortari, Sergio Robertohttp://lattes.cnpq.br/7784609477475171http://lattes.cnpq.br/4482737960721680Knorr, Camila de Lellis100600000000600eea59c2f-771c-4819-8dae-52d7ca97a3554ab15b54-3c1a-4b3e-94dd-f17db68c24058fd7d402-38cb-487a-ae04-60b751dc48d6a33c2787-11dc-4032-8dda-91a38ea80867a9ee5e70-810a-4fbb-8a1f-0e0aaf8d83f3ebb296a1-1569-43d1-8946-7cc7e3bec814reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2014_KNORR_CAMILA.pdfTES_PPGQUÍMICA_2014_KNORR_CAMILA.pdfTese de Doutoradoapplication/pdf931574http://repositorio.ufsm.br/bitstream/1/11988/1/TES_PPGQU%c3%8dMICA_2014_KNORR_CAMILA.pdf15ab54dd195b4a7b53fc159cac239940MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico |
title |
Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico |
spellingShingle |
Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico Knorr, Camila de Lellis Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico |
title_full |
Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico |
title_fullStr |
Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico |
title_full_unstemmed |
Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico |
title_sort |
Avaliação de métodos de preparo de amostras para posterior determinação de contaminantes inorgânicos em cápsulas de uso farmacêutico |
author |
Knorr, Camila de Lellis |
author_facet |
Knorr, Camila de Lellis |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Flores, Érico Marlon de Moraes |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/7167629055579212 |
dc.contributor.referee1.fl_str_mv |
Costa, Adilson Ben da |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/2604778196819181 |
dc.contributor.referee2.fl_str_mv |
Mello, Paola de Azevedo |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/2189500441942469 |
dc.contributor.referee3.fl_str_mv |
Dressler, Valderi Luiz |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/4054740296547580 |
dc.contributor.referee4.fl_str_mv |
Mortari, Sergio Roberto |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/7784609477475171 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/4482737960721680 |
dc.contributor.author.fl_str_mv |
Knorr, Camila de Lellis |
contributor_str_mv |
Flores, Érico Marlon de Moraes Costa, Adilson Ben da Mello, Paola de Azevedo Dressler, Valderi Luiz Mortari, Sergio Roberto |
dc.subject.por.fl_str_mv |
Química analítica |
topic |
Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, sample preparation methods were proposed, microwave-induced combustion (MIC) and microwave-assisted wet digestion (MAWD), for further Br, Cl, Cr, Cu, I and Mn determination in pharmaceutical capsules. For Cl, Br and I determination, ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) were used. The ICP-MS technique was also used for Cr, Cu and Mn determination, as well as graphite furnace atomic absorption spectrometry (GF AAS) and by solid sampling graphite furnace atomic absorption spectrometry (SS GF AAS). For MAWD digestion, it was possible to digest 300 mg samples, whereas in MIC up to 500 mg of sample were used. Also, MIC digestion allowed the digestion using diluted nitric acid for all elements, except for Br and I which require diluted alkaline solution. The carbon content was determined in samples after decomposition in order to evaluate the efficiency of decomposition. Sample decomposition was complete for all sample preparation methods applied, since the carbon content in MAWD solutions was 60 mg L-1 and it was lower than the limit of detection (10 mg L-1) for MIC solutions. Certified reference material of whole milk powder was used to evaluate the accuracy of MIC digestion and the agreement to certified values was between 94 and 102%. In conclusion, the investigated sample preparation methods were suitable to pharmaceutical capsules digestion as well as for the determination techniques. Also, chlorine recovery was possible with diluted acid solutions in MIC digestion. |
publishDate |
2014 |
dc.date.issued.fl_str_mv |
2014 |
dc.date.accessioned.fl_str_mv |
2017-11-08T12:35:23Z |
dc.date.available.fl_str_mv |
2017-11-08T12:35:23Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/11988 |
url |
http://repositorio.ufsm.br/handle/1/11988 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
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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 |
reponame:Biblioteca Digital de Teses e Dissertações do UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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