ExtraÃÃo, caracterizaÃÃo e modificaÃÃo quÃmica da pectina do melÃo caipira (Cucumis melo var. acidulus)
Autor(a) principal: | |
---|---|
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. |
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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 Cearà |
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 Cearà |
dc.source.none.fl_str_mv |
reponame:Biblioteca Digital de Teses e Dissertações da UFC instname:Universidade Federal do Ceará instacron:UFC |
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Biblioteca Digital de Teses e Dissertações da UFC |
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Biblioteca Digital de Teses e Dissertações da UFC |
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Universidade Federal do Ceará |
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UFC |
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UFC |
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mail@mail.com |
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