ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)

Detalhes bibliográficos
Autor(a) principal: Andrà Luiz Nascimento de Sousa
Data de Publicação: 2016
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Biblioteca Digital de Teses e Dissertações da UFC
Texto Completo: http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=16241
Resumo: In this work the extraction of substances from the common melon (Cucumis melo var. Acidulus) was carried out, which has more specific application in both, the food industry, as in the pharmaceutical and cosmetic industry, becoming more valuable than the fruit in natura. The objective of this study was to extract, quantify, characterize and modify chemically by sulfation pectin the common melon (Cucumis melo var. acidulus). The extractions were performed in neutral, acidic and basic conditions, with yields of 8%, 10.8% and 14%, respectively. In addition to the Elementary Analysis, pectin extracted with acid, it was characterized by nuclear magnetic resonance of carbon (13C NMR) and Hydrogen (1H NMR), Potentiometric Titration, Spectroscopy in the Infrared (FT-IR), Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), hermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), Gel Permeation Chromatography (GPC), Rheology and Zeta Potential. Some of these analyzes were not performed for samples extracted in alkaline, neutral and sulfated acid, as well as for commercial use sample, for which the analysis depended on the purpose for which it was proposed, is it to determine a specific feature the material and the degree of esterification (DE) or to identify overall change in polymer structure such as sulfation. The 13C-NMR showed peaks characteristic of galacturonic acid. The FT-IR and potentiometric titration permitted the calculation of the degree of esterification (DE) of acidic, basic, neutral and sulfated samples and also a commercial sample from Sigma Aldrich; GE results of the samples obtained by these techniques were compared, showing that the samples are acidic and neutral low GE. The result of GE acid sample was also obtained by 1H NMR, confirming its low GE condition. The SEM of the sample showed particles with acidic spherical structure with surface flattening, typical drying spray dried, suggesting potential application in drug encapsulation. The XRD revealed that the material has amorphous character, an increase of crystallinity after chemical modification. The TGA technique revealed the pectin degradation in three stages. The DSC curve showed an endothermic peak at 150 ÂC and an exotherm at 245ÂC for the loss of water and the main step of breakdown of the material, respectively. The molecular weight of the acid sample, determined by GPC, showed values of typical polymeric materials 4.5 x 105 g/mol, consistent with pectins. The rheological study revealed the shear-thinning property of pectin solution.
id UFC_99f70602ee208fdd22afcf2f6964450c
oai_identifier_str oai:www.teses.ufc.br:10615
network_acronym_str UFC
network_name_str Biblioteca Digital de Teses e Dissertações da UFC
spelling info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)Extraction , characterization and chemical modification of pectin hick melon (Cucumis melo var. acidulus)2016-10-09NÃgila Maria Pontes Silva Ricardo11279281391http://lattes.cnpq.br/6703037457253125SÃnia Maria Costa Siqueira00000000041http://lattes.cnpq.br/3732815540670292Tamara GonÃalves AraÃjo770 212 58372 http://lattes.cnpq.br/956725811784213357530955349http://lattes.cnpq.br/4524667886648783Andrà Luiz Nascimento de SousaUniversidade Federal do CearÃPrograma de PÃs-GraduaÃÃo em QuÃmica UFCBRMelÃo Pectina InfravermelhoRMNQUIMICAIn this work the extraction of substances from the common melon (Cucumis melo var. Acidulus) was carried out, which has more specific application in both, the food industry, as in the pharmaceutical and cosmetic industry, becoming more valuable than the fruit in natura. The objective of this study was to extract, quantify, characterize and modify chemically by sulfation pectin the common melon (Cucumis melo var. acidulus). The extractions were performed in neutral, acidic and basic conditions, with yields of 8%, 10.8% and 14%, respectively. In addition to the Elementary Analysis, pectin extracted with acid, it was characterized by nuclear magnetic resonance of carbon (13C NMR) and Hydrogen (1H NMR), Potentiometric Titration, Spectroscopy in the Infrared (FT-IR), Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), hermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), Gel Permeation Chromatography (GPC), Rheology and Zeta Potential. Some of these analyzes were not performed for samples extracted in alkaline, neutral and sulfated acid, as well as for commercial use sample, for which the analysis depended on the purpose for which it was proposed, is it to determine a specific feature the material and the degree of esterification (DE) or to identify overall change in polymer structure such as sulfation. The 13C-NMR showed peaks characteristic of galacturonic acid. The FT-IR and potentiometric titration permitted the calculation of the degree of esterification (DE) of acidic, basic, neutral and sulfated samples and also a commercial sample from Sigma Aldrich; GE results of the samples obtained by these techniques were compared, showing that the samples are acidic and neutral low GE. The result of GE acid sample was also obtained by 1H NMR, confirming its low GE condition. The SEM of the sample showed particles with acidic spherical structure with surface flattening, typical drying spray dried, suggesting potential application in drug encapsulation. The XRD revealed that the material has amorphous character, an increase of crystallinity after chemical modification. The TGA technique revealed the pectin degradation in three stages. The DSC curve showed an endothermic peak at 150 ÂC and an exotherm at 245ÂC for the loss of water and the main step of breakdown of the material, respectively. The molecular weight of the acid sample, determined by GPC, showed values of typical polymeric materials 4.5 x 105 g/mol, consistent with pectins. The rheological study revealed the shear-thinning property of pectin solution.Neste trabalho foi feita a extraÃÃo de substÃncias presentes no melÃo caipira (Cucumis melo var. acidulus) que tenham aplicaÃÃo mais especÃfica tanto na indÃstria alimentÃcia, quanto na indÃstria farmacÃutica e cosmÃtica, sendo, portanto, de maior valor comercial que os frutos in natura. O objetivo deste trabalho foi o de extrair, quantificar, caracterizar e modificar quimicamente por sulfataÃÃo a pectina do melÃo caipira (Cucumis melo var. acidulus). As extraÃÃes foram feitas em meio neutro, bÃsico e Ãcido, apresentando rendimentos de 8%, 10,8% e 14%, respectivamente. AlÃm da anÃlise elementar da pectina extraÃda em meio Ãcido, esta foi caracterizada por RessonÃncia MagnÃtica Nuclear do Carbono (RMN 13C) e do HidrogÃnio (RMN 1H), TitulaÃÃo PotenciomÃtrica, espectroscopia na regiÃo do infravermelho (FT-IR), Microscopia EletrÃnica de Varredura (MEV), DifraÃÃo de Raios-x (DRX), AnÃlise TermogravimÃtrica (TGA), Calorimetria ExploratÃria Diferencial (DSC), Cromatografia de PermeaÃÃo em Gel (GPC), Reologia e Potencial Zeta. Algumas dessas anÃlises nÃo foram realizadas para as amostras extraÃdas em meio bÃsico, neutro e a Ãcida sulfatada, bem como, para a amostra de uso comercial, para as quais, as anÃlises dependeram da finalidade a que se propunha, seja para determinar alguma caracterÃstica especÃfica do material como o Grau de EsterificaÃÃo (GE), seja para identificar mudanÃa geral na estrutura do polÃmero como a sulfataÃÃo. O RMN 13C revelou picos caracterÃsticos de Ãcido galacturÃnico. O FT-IR e a TitulaÃÃo PotenciomÃtrica permitiram o cÃlculo do Grau de EsterificaÃÃo (GE) das amostras Ãcida, bÃsica, neutra, sulfatada e tambÃm de uma amostra comercial da Sigma Aldrich; o resultado de GE das amostras, obtidos por essas tÃcnicas, foram comparados entre si, mostrando que as amostras Ãcida e neutra sÃo de baixo GE.O resultado de GE da amostra Ãcida tambÃm foi obtido por RMN 1H,confirmando sua condiÃÃo de baixo GE. O MEV da amostra Ãcida revelou partÃculas com estrutura esfÃrica com achatamentos superficiais, tÃpicos de secagem em spray dried, sugerindo potencial aplicaÃÃo em encapsulaÃÃo de fÃrmacos. A DRX revelou que o material apresenta carÃter amorfo, com aumento de cristalinidade apÃs modificaÃÃo quÃmica. A tÃcnica de TGA revelou os estÃgios de degradaÃÃo da pectina em trÃs etapas. A curva de DSC apresentou um pico endotÃrmico em 150 ÂC e um exotÃrmico em 245 ÂC, relativos à perda de Ãgua e à principal etapa de degradaÃÃo do material, respectivamente. A massa molecular da amostra Ãcida, determinada por GPC, apresentou valores tÃpicos de materiais polimÃricos 4,5 x 105 g/mol, condizentes com pectinas. O estudo reolÃgico revelou a propriedade pseudoplÃstica da soluÃÃo de pectina.http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=16241application/pdfinfo:eu-repo/semantics/openAccessporreponame:Biblioteca Digital de Teses e Dissertações da UFCinstname:Universidade Federal do Cearáinstacron:UFC2019-01-21T11:30:01Zmail@mail.com -
dc.title.pt.fl_str_mv ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
dc.title.alternative..fl_str_mv Extraction , characterization and chemical modification of pectin hick melon (Cucumis melo var. acidulus)
title ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
spellingShingle ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
Andrà Luiz Nascimento de Sousa
MelÃo
Pectina
Infravermelho
RMN
QUIMICA
title_short ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
title_full ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
title_fullStr ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
title_full_unstemmed ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
title_sort ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
author Andrà Luiz Nascimento de Sousa
author_facet Andrà Luiz Nascimento de Sousa
author_role author
dc.contributor.advisor1.fl_str_mv NÃgila Maria Pontes Silva Ricardo
dc.contributor.advisor1ID.fl_str_mv 11279281391
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/6703037457253125
dc.contributor.referee1.fl_str_mv SÃnia Maria Costa Siqueira
dc.contributor.referee1ID.fl_str_mv 00000000041
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/3732815540670292
dc.contributor.referee2.fl_str_mv Tamara GonÃalves AraÃjo
dc.contributor.referee2ID.fl_str_mv 770 212 58372
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/9567258117842133
dc.contributor.authorID.fl_str_mv 57530955349
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/4524667886648783
dc.contributor.author.fl_str_mv Andrà Luiz Nascimento de Sousa
contributor_str_mv NÃgila Maria Pontes Silva Ricardo
SÃnia Maria Costa Siqueira
Tamara GonÃalves AraÃjo
dc.subject.por.fl_str_mv MelÃo
Pectina
Infravermelho
RMN
topic MelÃo
Pectina
Infravermelho
RMN
QUIMICA
dc.subject.cnpq.fl_str_mv QUIMICA
dc.description.abstract.por.fl_txt_mv In this work the extraction of substances from the common melon (Cucumis melo var. Acidulus) was carried out, which has more specific application in both, the food industry, as in the pharmaceutical and cosmetic industry, becoming more valuable than the fruit in natura. The objective of this study was to extract, quantify, characterize and modify chemically by sulfation pectin the common melon (Cucumis melo var. acidulus). The extractions were performed in neutral, acidic and basic conditions, with yields of 8%, 10.8% and 14%, respectively. In addition to the Elementary Analysis, pectin extracted with acid, it was characterized by nuclear magnetic resonance of carbon (13C NMR) and Hydrogen (1H NMR), Potentiometric Titration, Spectroscopy in the Infrared (FT-IR), Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), hermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), Gel Permeation Chromatography (GPC), Rheology and Zeta Potential. Some of these analyzes were not performed for samples extracted in alkaline, neutral and sulfated acid, as well as for commercial use sample, for which the analysis depended on the purpose for which it was proposed, is it to determine a specific feature the material and the degree of esterification (DE) or to identify overall change in polymer structure such as sulfation. The 13C-NMR showed peaks characteristic of galacturonic acid. The FT-IR and potentiometric titration permitted the calculation of the degree of esterification (DE) of acidic, basic, neutral and sulfated samples and also a commercial sample from Sigma Aldrich; GE results of the samples obtained by these techniques were compared, showing that the samples are acidic and neutral low GE. The result of GE acid sample was also obtained by 1H NMR, confirming its low GE condition. The SEM of the sample showed particles with acidic spherical structure with surface flattening, typical drying spray dried, suggesting potential application in drug encapsulation. The XRD revealed that the material has amorphous character, an increase of crystallinity after chemical modification. The TGA technique revealed the pectin degradation in three stages. The DSC curve showed an endothermic peak at 150 ÂC and an exotherm at 245ÂC for the loss of water and the main step of breakdown of the material, respectively. The molecular weight of the acid sample, determined by GPC, showed values of typical polymeric materials 4.5 x 105 g/mol, consistent with pectins. The rheological study revealed the shear-thinning property of pectin solution.
Neste trabalho foi feita a extraÃÃo de substÃncias presentes no melÃo caipira (Cucumis melo var. acidulus) que tenham aplicaÃÃo mais especÃfica tanto na indÃstria alimentÃcia, quanto na indÃstria farmacÃutica e cosmÃtica, sendo, portanto, de maior valor comercial que os frutos in natura. O objetivo deste trabalho foi o de extrair, quantificar, caracterizar e modificar quimicamente por sulfataÃÃo a pectina do melÃo caipira (Cucumis melo var. acidulus). As extraÃÃes foram feitas em meio neutro, bÃsico e Ãcido, apresentando rendimentos de 8%, 10,8% e 14%, respectivamente. AlÃm da anÃlise elementar da pectina extraÃda em meio Ãcido, esta foi caracterizada por RessonÃncia MagnÃtica Nuclear do Carbono (RMN 13C) e do HidrogÃnio (RMN 1H), TitulaÃÃo PotenciomÃtrica, espectroscopia na regiÃo do infravermelho (FT-IR), Microscopia EletrÃnica de Varredura (MEV), DifraÃÃo de Raios-x (DRX), AnÃlise TermogravimÃtrica (TGA), Calorimetria ExploratÃria Diferencial (DSC), Cromatografia de PermeaÃÃo em Gel (GPC), Reologia e Potencial Zeta. Algumas dessas anÃlises nÃo foram realizadas para as amostras extraÃdas em meio bÃsico, neutro e a Ãcida sulfatada, bem como, para a amostra de uso comercial, para as quais, as anÃlises dependeram da finalidade a que se propunha, seja para determinar alguma caracterÃstica especÃfica do material como o Grau de EsterificaÃÃo (GE), seja para identificar mudanÃa geral na estrutura do polÃmero como a sulfataÃÃo. O RMN 13C revelou picos caracterÃsticos de Ãcido galacturÃnico. O FT-IR e a TitulaÃÃo PotenciomÃtrica permitiram o cÃlculo do Grau de EsterificaÃÃo (GE) das amostras Ãcida, bÃsica, neutra, sulfatada e tambÃm de uma amostra comercial da Sigma Aldrich; o resultado de GE das amostras, obtidos por essas tÃcnicas, foram comparados entre si, mostrando que as amostras Ãcida e neutra sÃo de baixo GE.O resultado de GE da amostra Ãcida tambÃm foi obtido por RMN 1H,confirmando sua condiÃÃo de baixo GE. O MEV da amostra Ãcida revelou partÃculas com estrutura esfÃrica com achatamentos superficiais, tÃpicos de secagem em spray dried, sugerindo potencial aplicaÃÃo em encapsulaÃÃo de fÃrmacos. A DRX revelou que o material apresenta carÃter amorfo, com aumento de cristalinidade apÃs modificaÃÃo quÃmica. A tÃcnica de TGA revelou os estÃgios de degradaÃÃo da pectina em trÃs etapas. A curva de DSC apresentou um pico endotÃrmico em 150 ÂC e um exotÃrmico em 245 ÂC, relativos à perda de Ãgua e à principal etapa de degradaÃÃo do material, respectivamente. A massa molecular da amostra Ãcida, determinada por GPC, apresentou valores tÃpicos de materiais polimÃricos 4,5 x 105 g/mol, condizentes com pectinas. O estudo reolÃgico revelou a propriedade pseudoplÃstica da soluÃÃo de pectina.
description In this work the extraction of substances from the common melon (Cucumis melo var. Acidulus) was carried out, which has more specific application in both, the food industry, as in the pharmaceutical and cosmetic industry, becoming more valuable than the fruit in natura. The objective of this study was to extract, quantify, characterize and modify chemically by sulfation pectin the common melon (Cucumis melo var. acidulus). The extractions were performed in neutral, acidic and basic conditions, with yields of 8%, 10.8% and 14%, respectively. In addition to the Elementary Analysis, pectin extracted with acid, it was characterized by nuclear magnetic resonance of carbon (13C NMR) and Hydrogen (1H NMR), Potentiometric Titration, Spectroscopy in the Infrared (FT-IR), Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), hermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), Gel Permeation Chromatography (GPC), Rheology and Zeta Potential. Some of these analyzes were not performed for samples extracted in alkaline, neutral and sulfated acid, as well as for commercial use sample, for which the analysis depended on the purpose for which it was proposed, is it to determine a specific feature the material and the degree of esterification (DE) or to identify overall change in polymer structure such as sulfation. The 13C-NMR showed peaks characteristic of galacturonic acid. The FT-IR and potentiometric titration permitted the calculation of the degree of esterification (DE) of acidic, basic, neutral and sulfated samples and also a commercial sample from Sigma Aldrich; GE results of the samples obtained by these techniques were compared, showing that the samples are acidic and neutral low GE. The result of GE acid sample was also obtained by 1H NMR, confirming its low GE condition. The SEM of the sample showed particles with acidic spherical structure with surface flattening, typical drying spray dried, suggesting potential application in drug encapsulation. The XRD revealed that the material has amorphous character, an increase of crystallinity after chemical modification. The TGA technique revealed the pectin degradation in three stages. The DSC curve showed an endothermic peak at 150 ÂC and an exotherm at 245ÂC for the loss of water and the main step of breakdown of the material, respectively. The molecular weight of the acid sample, determined by GPC, showed values of typical polymeric materials 4.5 x 105 g/mol, consistent with pectins. The rheological study revealed the shear-thinning property of pectin solution.
publishDate 2016
dc.date.issued.fl_str_mv 2016-10-09
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
status_str publishedVersion
format masterThesis
dc.identifier.uri.fl_str_mv http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=16241
url http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=16241
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal do CearÃ
dc.publisher.program.fl_str_mv Programa de PÃs-GraduaÃÃo em QuÃmica
dc.publisher.initials.fl_str_mv UFC
dc.publisher.country.fl_str_mv BR
publisher.none.fl_str_mv Universidade Federal do CearÃ
dc.source.none.fl_str_mv reponame:Biblioteca Digital de Teses e Dissertações da UFC
instname:Universidade Federal do Ceará
instacron:UFC
reponame_str Biblioteca Digital de Teses e Dissertações da UFC
collection Biblioteca Digital de Teses e Dissertações da UFC
instname_str Universidade Federal do Ceará
instacron_str UFC
institution UFC
repository.name.fl_str_mv -
repository.mail.fl_str_mv mail@mail.com
_version_ 1643295220286095360