Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica

Detalhes bibliográficos
Autor(a) principal: Silva, Leila Melo da
Data de Publicação: 2019
Tipo de documento: Tese
Idioma: por
Título da fonte: Repositório Institucional da UFS
Texto Completo: http://ri.ufs.br/jspui/handle/riufs/11303
Resumo: The Mg2+, Mn2+ and Sr2+ ions are of great biological interest in association with hydroxyapatite (HA) for inducing positive cellular responses in bone regeneration. However, these ions are difficult to stabilize in the crystal lattice of HA synthesized by co-precipitation, generally inducing phase transformations during thermal treatments above 800°C. The new phases are rarely taken into account when these materials are tested with cells. In many cases, the effects attributed to one element in substituted HA are mixed with those caused by the presence of unaccounted phases. Thus, the objective of this work was to isolate the effects of the ions over the cells from those caused by the inherent phase transformations in the substituted HA systems. At the same time, to propose a differentiated method for the insertion of these ions into a pre-synthesized HA via ion exchange assisted by microwave radiation. Samples of pure HA and containing the different ions were synthesized by co-precipitation and physic-chemically characterized by wavelength disperse X- ray fluorescence (WDXRF), X-ray diffraction (XRD) with Rietveld refinement and Fourier transform infrared spectroscopy (FTIR), before and after calcination at 1000 °C. Calcined samples were assayed with mouse pre-osteoblastic cells (MC3T3-E1). The samples used in the ion exchange assays were physic-chemically characterized to evaluate the insertion of the elements in the HA lattice. The addition of Mg2+, Mn2+ and Sr2+ ions in the HA lattice, through co-precipitation, promoted the formation of the CaO, MgO and Mn3O4 phases, after calcination at 1000 °C, as well as changes in the unit cell volume. It was observed that Mg2+ ions stimulated the differentiation of the pre-osteoblasts even when segregated from the HA structure as MgO. However, the presence of MgO appeared to retard cell proliferation. At the same time, Mn2+ ions increased cell proliferation and induced the production of high levels of alkaline phosphatase (ALP), regardless whether they were inserted into the HA structure or segregated in the form of Mn3O4. The presence of Sr2+ in the HA lattice did not affect cell behavior, since both proliferation and ALP production were comparable to those observed for pure HA. Regarding the alternative method of ion exchange for inserting the ions into the HA, the microwave radiation heating considerably increased the ion concentration in the HA samples compared to the conventional heating. However, that most of the ions remained in a hydrated layer onto the crystal surface, without significant diffusion to the bulk.
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spelling Silva, Leila Melo daSantos, Euler Araujo dos2019-06-04T23:13:17Z2019-06-04T23:13:17Z2019-03-20SILVA, Leila Melo da. Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica. 2019. 116 f. Tese (Doutorado em Ciência e Engenharia de Materiais) - Universidade Federal de Sergipe, São Cristóvão, SE, 2019.http://ri.ufs.br/jspui/handle/riufs/11303The Mg2+, Mn2+ and Sr2+ ions are of great biological interest in association with hydroxyapatite (HA) for inducing positive cellular responses in bone regeneration. However, these ions are difficult to stabilize in the crystal lattice of HA synthesized by co-precipitation, generally inducing phase transformations during thermal treatments above 800°C. The new phases are rarely taken into account when these materials are tested with cells. In many cases, the effects attributed to one element in substituted HA are mixed with those caused by the presence of unaccounted phases. Thus, the objective of this work was to isolate the effects of the ions over the cells from those caused by the inherent phase transformations in the substituted HA systems. At the same time, to propose a differentiated method for the insertion of these ions into a pre-synthesized HA via ion exchange assisted by microwave radiation. Samples of pure HA and containing the different ions were synthesized by co-precipitation and physic-chemically characterized by wavelength disperse X- ray fluorescence (WDXRF), X-ray diffraction (XRD) with Rietveld refinement and Fourier transform infrared spectroscopy (FTIR), before and after calcination at 1000 °C. Calcined samples were assayed with mouse pre-osteoblastic cells (MC3T3-E1). The samples used in the ion exchange assays were physic-chemically characterized to evaluate the insertion of the elements in the HA lattice. The addition of Mg2+, Mn2+ and Sr2+ ions in the HA lattice, through co-precipitation, promoted the formation of the CaO, MgO and Mn3O4 phases, after calcination at 1000 °C, as well as changes in the unit cell volume. It was observed that Mg2+ ions stimulated the differentiation of the pre-osteoblasts even when segregated from the HA structure as MgO. However, the presence of MgO appeared to retard cell proliferation. At the same time, Mn2+ ions increased cell proliferation and induced the production of high levels of alkaline phosphatase (ALP), regardless whether they were inserted into the HA structure or segregated in the form of Mn3O4. The presence of Sr2+ in the HA lattice did not affect cell behavior, since both proliferation and ALP production were comparable to those observed for pure HA. Regarding the alternative method of ion exchange for inserting the ions into the HA, the microwave radiation heating considerably increased the ion concentration in the HA samples compared to the conventional heating. However, that most of the ions remained in a hydrated layer onto the crystal surface, without significant diffusion to the bulk.Os íons Mg2+, Mn2+ e Sr2+ são de grande interesse biológico em associação à hidroxiapatita (HA) por induzir respostas celulares que promovem regeneração óssea. No entanto, esses íons são de difícil estabilização na rede cristalina de HAs obtidas por co-precipitação, as quais podem sofrer transformações de fase em tratamentos térmicos acima de 800°C. As novas fases são raramente levadas em conta quando se avaliam os efeitos desses íons sobre o comportamento celular. Em muitos casos, os efeitos atribuídos a um íon são misturados com aqueles causados pela presença de outras fases não contabilizadas. Assim, o objetivo deste trabalho foi compreender como ocorre a estabilização desses íons na rede de uma HA, isolando seus efeitos sobre as células, daqueles causados por transformações de fase inerentes aos sistemas de HA substituídas. Ao mesmo tempo, propor um método diferenciado para a inserção desses íons em uma HA pré-sintetizada via troca iônica assistida por radiação micro-ondas. Para tanto, amostras de HA pura e contendo os diferentes íons foram sintetizadas via co-precipitação e caracterizadas físico-quimicamente por espectroscopia de fluorescência de raios X por dispersão de comprimento de onda (WDXRF), difração de raios X (XRD) com refinamento Rietveld e espectroscopia no infravermelho por transformada de Fourier (FTIR), antes e após calcinação a 1000°C. As amostras calcinadas foram testadas com células pré-osteoblásticas de camundongos (MC3T3-E1). As amostras ensaiadas em troca iônica também foram caracterizadas físico-quimicamente, para se avaliar o nível de entrada dos elementos na rede da HA. A entrada dos íons Mg2+, Mn2+ e Sr2+ na rede da HA, via co-precipitação, promoveu a formação das fases CaO, MgO e Mn3O4, após calcinação a 1000°C, além de modificações no volume da célula unitária. Observou-se que os íons Mg2+ estimularam a diferenciação dos pré-osteoblastos mesmo quando segregados da estrutura HA na forma de MgO. No entanto, a presença de MgO retardou a proliferação celular. Ao mesmo tempo, os íons Mn2+ aumentaram a proliferação celular e induziram a produção de altos níveis de fosfatase alcalina (ALP), independentemente de estarem inseridos na estrutura de HA ou estarem segregados na forma de Mn3O4. A presença de Sr2+ na rede da HA não afetou o comportamento celular, pois tanto a proliferação quanto a produção de ALP foram comparáveis àquelas observadas para a HA pura. Em relação ao método alternativo de troca-iônica para inserção dos íons sem indução de transformações de fase, o aquecimento via radiação micro-ondas aumentou a concentração dos íons nas amostras de HA, em comparação ao aquecimento convencional. No entanto, a maior parte dos íons permaneceu numa camada hidratada da superfície dos cristais, sem difusão significativa para o bulk.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESSão Cristóvão, SEporCiência dos materiaisHidroxiapatitaTroca iônicaOsteoblastosPrecipitação (Química)DopagemHydroxyapatiteDopingOsteoblastPrecipitationIon exchangeENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICAEfeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônicaEffect of the simultaneous insertion of Mg2+, Mn2+ AND Sr2+ on hydroxyapatite in precipitation and ion exchange processesinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisPós-Graduação em Ciência e Engenharia de MateriaisUFSreponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSinfo:eu-repo/semantics/openAccessTEXTLEILA_MELO_SILVA.pdf.txtLEILA_MELO_SILVA.pdf.txtExtracted texttext/plain187086https://ri.ufs.br/jspui/bitstream/riufs/11303/3/LEILA_MELO_SILVA.pdf.txte61cc19b2bb096bb94068f3ff3bc7271MD53THUMBNAILLEILA_MELO_SILVA.pdf.jpgLEILA_MELO_SILVA.pdf.jpgGenerated Thumbnailimage/jpeg1295https://ri.ufs.br/jspui/bitstream/riufs/11303/4/LEILA_MELO_SILVA.pdf.jpg1b2d68f847052c58736225041adaebe4MD54LICENSElicense.txtlicense.txttext/plain; charset=utf-81475https://ri.ufs.br/jspui/bitstream/riufs/11303/1/license.txt098cbbf65c2c15e1fb2e49c5d306a44cMD51ORIGINALLEILA_MELO_SILVA.pdfLEILA_MELO_SILVA.pdfapplication/pdf5881454https://ri.ufs.br/jspui/bitstream/riufs/11303/2/LEILA_MELO_SILVA.pdfa7f53598aa3fdfa548064362846f6ac2MD52riufs/113032019-06-04 20:13:17.837oai:ufs.br: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Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2019-06-04T23:13:17Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false
dc.title.pt_BR.fl_str_mv Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica
dc.title.alternative.por.fl_str_mv Effect of the simultaneous insertion of Mg2+, Mn2+ AND Sr2+ on hydroxyapatite in precipitation and ion exchange processes
title Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica
spellingShingle Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica
Silva, Leila Melo da
Ciência dos materiais
Hidroxiapatita
Troca iônica
Osteoblastos
Precipitação (Química)
Dopagem
Hydroxyapatite
Doping
Osteoblast
Precipitation
Ion exchange
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
title_short Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica
title_full Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica
title_fullStr Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica
title_full_unstemmed Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica
title_sort Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica
author Silva, Leila Melo da
author_facet Silva, Leila Melo da
author_role author
dc.contributor.author.fl_str_mv Silva, Leila Melo da
dc.contributor.advisor1.fl_str_mv Santos, Euler Araujo dos
contributor_str_mv Santos, Euler Araujo dos
dc.subject.por.fl_str_mv Ciência dos materiais
Hidroxiapatita
Troca iônica
Osteoblastos
Precipitação (Química)
Dopagem
topic Ciência dos materiais
Hidroxiapatita
Troca iônica
Osteoblastos
Precipitação (Química)
Dopagem
Hydroxyapatite
Doping
Osteoblast
Precipitation
Ion exchange
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
dc.subject.eng.fl_str_mv Hydroxyapatite
Doping
Osteoblast
Precipitation
Ion exchange
dc.subject.cnpq.fl_str_mv ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA
description The Mg2+, Mn2+ and Sr2+ ions are of great biological interest in association with hydroxyapatite (HA) for inducing positive cellular responses in bone regeneration. However, these ions are difficult to stabilize in the crystal lattice of HA synthesized by co-precipitation, generally inducing phase transformations during thermal treatments above 800°C. The new phases are rarely taken into account when these materials are tested with cells. In many cases, the effects attributed to one element in substituted HA are mixed with those caused by the presence of unaccounted phases. Thus, the objective of this work was to isolate the effects of the ions over the cells from those caused by the inherent phase transformations in the substituted HA systems. At the same time, to propose a differentiated method for the insertion of these ions into a pre-synthesized HA via ion exchange assisted by microwave radiation. Samples of pure HA and containing the different ions were synthesized by co-precipitation and physic-chemically characterized by wavelength disperse X- ray fluorescence (WDXRF), X-ray diffraction (XRD) with Rietveld refinement and Fourier transform infrared spectroscopy (FTIR), before and after calcination at 1000 °C. Calcined samples were assayed with mouse pre-osteoblastic cells (MC3T3-E1). The samples used in the ion exchange assays were physic-chemically characterized to evaluate the insertion of the elements in the HA lattice. The addition of Mg2+, Mn2+ and Sr2+ ions in the HA lattice, through co-precipitation, promoted the formation of the CaO, MgO and Mn3O4 phases, after calcination at 1000 °C, as well as changes in the unit cell volume. It was observed that Mg2+ ions stimulated the differentiation of the pre-osteoblasts even when segregated from the HA structure as MgO. However, the presence of MgO appeared to retard cell proliferation. At the same time, Mn2+ ions increased cell proliferation and induced the production of high levels of alkaline phosphatase (ALP), regardless whether they were inserted into the HA structure or segregated in the form of Mn3O4. The presence of Sr2+ in the HA lattice did not affect cell behavior, since both proliferation and ALP production were comparable to those observed for pure HA. Regarding the alternative method of ion exchange for inserting the ions into the HA, the microwave radiation heating considerably increased the ion concentration in the HA samples compared to the conventional heating. However, that most of the ions remained in a hydrated layer onto the crystal surface, without significant diffusion to the bulk.
publishDate 2019
dc.date.accessioned.fl_str_mv 2019-06-04T23:13:17Z
dc.date.available.fl_str_mv 2019-06-04T23:13:17Z
dc.date.issued.fl_str_mv 2019-03-20
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/doctoralThesis
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dc.identifier.citation.fl_str_mv SILVA, Leila Melo da. Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica. 2019. 116 f. Tese (Doutorado em Ciência e Engenharia de Materiais) - Universidade Federal de Sergipe, São Cristóvão, SE, 2019.
dc.identifier.uri.fl_str_mv http://ri.ufs.br/jspui/handle/riufs/11303
identifier_str_mv SILVA, Leila Melo da. Efeitos da inserção simultânea dos íons Mg2+, Mn2+ e Sr2+ sobre hidroxiapatita em processo de precipitação e troca iônica. 2019. 116 f. Tese (Doutorado em Ciência e Engenharia de Materiais) - Universidade Federal de Sergipe, São Cristóvão, SE, 2019.
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