Quitosana sulfatada: caracterização e estudo da hemocompatibilidade

Detalhes bibliográficos
Ano de defesa: 2016
Autor(a) principal: Moraes, Anaftália Felismino
Orientador(a): Vieira, Rodrigo Silveira
Banca de defesa: Não Informado pela instituição
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Não Informado pela instituição
Programa de Pós-Graduação: Não Informado pela instituição
Departamento: Não Informado pela instituição
País: Não Informado pela instituição
Palavras-chave em Português:
Link de acesso: http://www.repositorio.ufc.br/handle/riufc/23214
Resumo: Medical devices designed to be used in contact with blood can induce several biological effects in the patient, such as the thrombus formation and complement system activation. An strategy to avoid these adverse effects is the coating of the surfaces with hemocompatible and not immunogenic polymers. This study aimed to develop sulfated chitosan films with hemocompatible characteristics for biomedical applications. Natural (NC) and sulfated chitosan (SC) films were characterized by Elemental Analysis, Infrared spectroscopy (FTIR-ATR), Proton and Carbon Nuclear Magnetic Resonance (1H e 13C-NMR), Viscometry, Gel Permeation Chromatography (GPC), Scanning Electron Microscopy with EDX (SEM/EDX), X-ray diffraction (XRD) and Thermogravimetric analysis (TGA). The films hemocompatibility was analyzed studying the globular protein adsorption (BSA and fibrinogen), platelet adhesion, anticoagulant activity and cytotoxicity by LDH (lactate dehydrogenase). The elemental analysis demonstrated the sulfur presence in the sulfated films. The FTIR-ATR results confirmed the sulfation reaction, with the appearance of two new bands at 1206cm -1 (S = O) and 794cm -1 (C-S-O), assigned at sulfur group. The film QS6 with the highest sulfation degree (GS =1.37) was selected to perform the following analyzes. The 1HNMR analysis showed deacetylation degree (DD) of 77% and 58% for the natural and sulfated chitosan, respectively. 13CNMR analysis showed that chitosan was partially sulfated, obtaining 2, N-3,6,O-sulfated chitosan. The mass molecular (MM) of QN and QS were 78.093 Da and 5.050 Da, respectively, determined by viscometry. Homogeneous and smooth surfaces were observed by SEM/EDX images. The XRD showed semi-crystalline peaks for natural chitosan, while an amorphous structure was observed for sulfated chitosan. The TGA analyses revealed a reduction in the thermal stability to sulfated chitosan compared to natural chitosan. The hemocompatibility results showed that chemical modification on chitosan chain was able to decrease the BSA (36.8%) and fibrinogen (20%) adsorption and mainly the platelet adhesion (93.7%) in relation to QN, either by SEM and optical microscopy images. Only the QS presented anticoagulant activity in the intrinsic pathway (72.15s, 200µg/mL) compared with the QN (26.57s, 200µg/mL). It was also observed atoxicity of the studied polymers. These results indicate that sulfated chitosan films have hemocompatibility properties promising to blood-materials devices.
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spelling Moraes, Anaftália FelisminoVieira, Rodrigo Silveira2017-06-12T14:30:21Z2017-06-12T14:30:21Z2016MORAES, A. F. Quitosana sulfatada: caracterização e estudo da hemocompatibilidade. 2016. 90 f. Dissertação (Mestrado em Engenharia Química)-Centro de Tecnologia, Universidade Federal do Ceará, Fortaleza, 2016.http://www.repositorio.ufc.br/handle/riufc/23214Medical devices designed to be used in contact with blood can induce several biological effects in the patient, such as the thrombus formation and complement system activation. An strategy to avoid these adverse effects is the coating of the surfaces with hemocompatible and not immunogenic polymers. This study aimed to develop sulfated chitosan films with hemocompatible characteristics for biomedical applications. Natural (NC) and sulfated chitosan (SC) films were characterized by Elemental Analysis, Infrared spectroscopy (FTIR-ATR), Proton and Carbon Nuclear Magnetic Resonance (1H e 13C-NMR), Viscometry, Gel Permeation Chromatography (GPC), Scanning Electron Microscopy with EDX (SEM/EDX), X-ray diffraction (XRD) and Thermogravimetric analysis (TGA). The films hemocompatibility was analyzed studying the globular protein adsorption (BSA and fibrinogen), platelet adhesion, anticoagulant activity and cytotoxicity by LDH (lactate dehydrogenase). The elemental analysis demonstrated the sulfur presence in the sulfated films. The FTIR-ATR results confirmed the sulfation reaction, with the appearance of two new bands at 1206cm -1 (S = O) and 794cm -1 (C-S-O), assigned at sulfur group. The film QS6 with the highest sulfation degree (GS =1.37) was selected to perform the following analyzes. The 1HNMR analysis showed deacetylation degree (DD) of 77% and 58% for the natural and sulfated chitosan, respectively. 13CNMR analysis showed that chitosan was partially sulfated, obtaining 2, N-3,6,O-sulfated chitosan. The mass molecular (MM) of QN and QS were 78.093 Da and 5.050 Da, respectively, determined by viscometry. Homogeneous and smooth surfaces were observed by SEM/EDX images. The XRD showed semi-crystalline peaks for natural chitosan, while an amorphous structure was observed for sulfated chitosan. The TGA analyses revealed a reduction in the thermal stability to sulfated chitosan compared to natural chitosan. The hemocompatibility results showed that chemical modification on chitosan chain was able to decrease the BSA (36.8%) and fibrinogen (20%) adsorption and mainly the platelet adhesion (93.7%) in relation to QN, either by SEM and optical microscopy images. Only the QS presented anticoagulant activity in the intrinsic pathway (72.15s, 200µg/mL) compared with the QN (26.57s, 200µg/mL). It was also observed atoxicity of the studied polymers. These results indicate that sulfated chitosan films have hemocompatibility properties promising to blood-materials devices.Dispositivos médicos de contato com o sangue podem induzir diversos efeitos biológicos no paciente, tais como a formação de trombos e ativação do sistema complemento. Uma estratégia para evitar esses efeitos adversos é o revestimento dessas superfícies com polímeros hemocompatíveis e não imunogênicos. Com isso, este estudo objetivou desenvolver filmes de quitosana sulfatada com propriedades hemocompatíveis para aplicações biomédicas. Filmes de quitosana natural (QN) e sulfatada (QS) foram caracterizados por Análise Elementar, espectroscopia de infravermelho (FTIR-ATR), Ressonância Magnética Nuclear de Próton e Carbono (1H e 13C-RMN), Viscosimetria, Cromatografia de Permeação em Gel (GPC), Microscopia Eletrônica de Varredura com Energia Dispersiva de raios-X (MEV/EDX), Difração de Raio-X (DRX) e Análise termogravimétrica (TGA). Para estudar a hemocompatibilidade dos filmes realizou-se o ensaio de adsorção de proteínas globulares (BSA e Fibrinogênio), adesão plaquetária, atividade anticoagulante e citotoxicidade por LDH (enzima lactato desidrogenase). Na análise elementar pode-se verificar a presença de enxofre nos filmes sulfatados. Através do FTIR-ATR pode-se confirmar a modificação com o surgimento de duas novas bandas em 1206 cm-1 (S=O) e 794 cm-1 (C-S-O), referentes a grupos sulfatos. O filme QS6 apresentou maior grau de sulfatação (GS=1.37) e foi selecionado para as análises subsequentes. A análise de RMN1H mostrou um grau de desacetilação (GD) de 77% e 58%, respectivamente para a QN e QS. Através da análise de RMN13C, observou-se uma quitosana parcialmente 2,N-3,6,O-sulfatada. A massa molecular (MM) das amostras foi 78.093 Da e 5.050 Da, para a QN e QS, respectivamente, determinadas por viscosimetria. Superfícies homogêneas e lisas foram observadas através das imagens do MEV/EDX. O difratograma mostrou picos semicristalinos para a QN e estrutura amorfa para a QS. Através da TGA, observou-se que a quitosana sulfatada teve uma redução da sua resistência térmica, comparada com a QN. Os resultados da hemocompatibilidade mostraram que a modificação química da quitosana foi capaz de reduzir a adsorção de BSA (36.8%) e fibrinogênio (20%) e principalmente a adesão plaquetária (93.7%) em relação à QN, observada nas imagens de MEV e microscopia óptica. Apenas a QS mostrou atividade anticoagulante na fase intrínseca (72.15s, 200µg/mL) em relação a QN (26.57s, 200µg/mL). Foi observado ainda a atoxicidade dos polímeros. Estes resultados indicaram que a QS apresentou características promissoras de hemocompatibilidade para dispositivos médicos de contato com o sangue.Engenharia químicaHemocompatibilidadeAtividade antitrombogênicaQuitosanaQuitosana sulfatada: caracterização e estudo da hemocompatibilidadeSulfated chitosan: characterization and hemocompatibility studyinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisporreponame:Repositório Institucional da Universidade Federal do Ceará (UFC)instname:Universidade Federal do Ceará (UFC)instacron:UFCinfo:eu-repo/semantics/openAccessORIGINAL2016_dis_afmoraes.pdf2016_dis_afmoraes.pdfapplication/pdf2876160http://repositorio.ufc.br/bitstream/riufc/23214/1/2016_dis_afmoraes.pdfccf2264487cf0c85c1acbd26da9fa14dMD51LICENSElicense.txtlicense.txttext/plain; charset=utf-81748http://repositorio.ufc.br/bitstream/riufc/23214/2/license.txt8a4605be74aa9ea9d79846c1fba20a33MD52riufc/232142022-02-23 11:12:45.798oai:repositorio.ufc.br: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Repositório InstitucionalPUBhttp://www.repositorio.ufc.br/ri-oai/requestbu@ufc.br || repositorio@ufc.bropendoar:2022-02-23T14:12:45Repositório Institucional da Universidade Federal do Ceará (UFC) - Universidade Federal do Ceará (UFC)false
dc.title.pt_BR.fl_str_mv Quitosana sulfatada: caracterização e estudo da hemocompatibilidade
dc.title.en.pt_BR.fl_str_mv Sulfated chitosan: characterization and hemocompatibility study
title Quitosana sulfatada: caracterização e estudo da hemocompatibilidade
spellingShingle Quitosana sulfatada: caracterização e estudo da hemocompatibilidade
Moraes, Anaftália Felismino
Engenharia química
Hemocompatibilidade
Atividade antitrombogênica
Quitosana
title_short Quitosana sulfatada: caracterização e estudo da hemocompatibilidade
title_full Quitosana sulfatada: caracterização e estudo da hemocompatibilidade
title_fullStr Quitosana sulfatada: caracterização e estudo da hemocompatibilidade
title_full_unstemmed Quitosana sulfatada: caracterização e estudo da hemocompatibilidade
title_sort Quitosana sulfatada: caracterização e estudo da hemocompatibilidade
author Moraes, Anaftália Felismino
author_facet Moraes, Anaftália Felismino
author_role author
dc.contributor.author.fl_str_mv Moraes, Anaftália Felismino
dc.contributor.advisor1.fl_str_mv Vieira, Rodrigo Silveira
contributor_str_mv Vieira, Rodrigo Silveira
dc.subject.por.fl_str_mv Engenharia química
Hemocompatibilidade
Atividade antitrombogênica
Quitosana
topic Engenharia química
Hemocompatibilidade
Atividade antitrombogênica
Quitosana
description Medical devices designed to be used in contact with blood can induce several biological effects in the patient, such as the thrombus formation and complement system activation. An strategy to avoid these adverse effects is the coating of the surfaces with hemocompatible and not immunogenic polymers. This study aimed to develop sulfated chitosan films with hemocompatible characteristics for biomedical applications. Natural (NC) and sulfated chitosan (SC) films were characterized by Elemental Analysis, Infrared spectroscopy (FTIR-ATR), Proton and Carbon Nuclear Magnetic Resonance (1H e 13C-NMR), Viscometry, Gel Permeation Chromatography (GPC), Scanning Electron Microscopy with EDX (SEM/EDX), X-ray diffraction (XRD) and Thermogravimetric analysis (TGA). The films hemocompatibility was analyzed studying the globular protein adsorption (BSA and fibrinogen), platelet adhesion, anticoagulant activity and cytotoxicity by LDH (lactate dehydrogenase). The elemental analysis demonstrated the sulfur presence in the sulfated films. The FTIR-ATR results confirmed the sulfation reaction, with the appearance of two new bands at 1206cm -1 (S = O) and 794cm -1 (C-S-O), assigned at sulfur group. The film QS6 with the highest sulfation degree (GS =1.37) was selected to perform the following analyzes. The 1HNMR analysis showed deacetylation degree (DD) of 77% and 58% for the natural and sulfated chitosan, respectively. 13CNMR analysis showed that chitosan was partially sulfated, obtaining 2, N-3,6,O-sulfated chitosan. The mass molecular (MM) of QN and QS were 78.093 Da and 5.050 Da, respectively, determined by viscometry. Homogeneous and smooth surfaces were observed by SEM/EDX images. The XRD showed semi-crystalline peaks for natural chitosan, while an amorphous structure was observed for sulfated chitosan. The TGA analyses revealed a reduction in the thermal stability to sulfated chitosan compared to natural chitosan. The hemocompatibility results showed that chemical modification on chitosan chain was able to decrease the BSA (36.8%) and fibrinogen (20%) adsorption and mainly the platelet adhesion (93.7%) in relation to QN, either by SEM and optical microscopy images. Only the QS presented anticoagulant activity in the intrinsic pathway (72.15s, 200µg/mL) compared with the QN (26.57s, 200µg/mL). It was also observed atoxicity of the studied polymers. These results indicate that sulfated chitosan films have hemocompatibility properties promising to blood-materials devices.
publishDate 2016
dc.date.issued.fl_str_mv 2016
dc.date.accessioned.fl_str_mv 2017-06-12T14:30:21Z
dc.date.available.fl_str_mv 2017-06-12T14:30:21Z
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dc.identifier.citation.fl_str_mv MORAES, A. F. Quitosana sulfatada: caracterização e estudo da hemocompatibilidade. 2016. 90 f. Dissertação (Mestrado em Engenharia Química)-Centro de Tecnologia, Universidade Federal do Ceará, Fortaleza, 2016.
dc.identifier.uri.fl_str_mv http://www.repositorio.ufc.br/handle/riufc/23214
identifier_str_mv MORAES, A. F. Quitosana sulfatada: caracterização e estudo da hemocompatibilidade. 2016. 90 f. Dissertação (Mestrado em Engenharia Química)-Centro de Tecnologia, Universidade Federal do Ceará, Fortaleza, 2016.
url http://www.repositorio.ufc.br/handle/riufc/23214
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