Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN
Ano de defesa: | 2018 |
---|---|
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 São Carlos
Câmpus São Carlos |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química - PPGQ
|
Departamento: |
Não Informado pela instituição
|
País: |
Não Informado pela instituição
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://repositorio.ufscar.br/handle/ufscar/10412 |
Resumo: | Acai is a widely consumed fruit in the North Region of Brazil and has gained consumers in other regions of the country and abroad. With the increasing acai pulp demand, quality control measures become necessary to improve its trading; however, there are some problems, such as the fast degradation of the pulp, microbiological contamination and no knowledge on the behavior of the organic compounds present in the pulp of fruits of different origins, growing, seasonality, transport and processing. This study describes the influence of seasonality, growing conditions and genotypic variations on the acai pulp from Belém - PA by 1H NMR combined with chemometric methods, and structural characterization of the chemical constituents by LC-DAD-SPE/NMR. This work was performed in 4 stages: I) Identification of the greatest number of organic compounds by 1D and 2D NMR, without the need for isolation; II) Attainment of the chemical profile by 1H NMR combined with the chemometric treatment of the pulp of the fruits of 31 genotypes cultivated under agronomic control (Embrapa Amazônia Oriental) and also of commercial samples (Belém-PA); III) Verification of the correlation between the 1H NMR chemical profile and the physical-chemical data measured in the same samples; and IV) Identification of the organic compounds present in the commercial acai pulp extracts obtained with an ASETM (accelerated solvent extractor), being the major compounds obtained by 1D and 2D NMR, and the minor ones by LC-DAD-SPE/NMR with time-slice as trapping mode. Tendencies in the distribution of the acai pulp samples were observed according to the type of growing (agronomic control x without control), seasonality (harvest season x inter-harvest season), genetic improvement, and the storage system used by the retailers from Belém, and the compounds responsible for such tendencies were identified. The great variability in the physical-chemical data of the evaluated pulps was verified and, thus, there was no correlation with the 1H NMR spectral data. The ASE provided the best extracts when compared to extracts obtained with the conventional method. Some aromatic compounds were isolated from the acai pulp methanolic extract by LC-DAD-SPE, and their structures were determined based on the analysis of 1D and 2D NMR, UV and MS experiments. This study showed the potential of the high-resolution NMR technique to obtain chemical information from the lyophilized acai pulp. The traditional analysis methods (physical-chemical ones) were not viable, since they did not provide good comprehension of the variations of the acai pulps. The ASE extractor was a good alternative to perform the clean-up and extraction of the organic compounds present in acai and the time-slice mode proved efficient in the isolation of compounds at low concentration present in the acai pulp methanolic extract. |
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Alves, Thayana da ConceiçãoFerreira, Antonio Gilbertohttp://lattes.cnpq.br/3676462220401452http://lattes.cnpq.br/03994345941908772018-08-29T13:35:27Z2018-08-29T13:35:27Z2018-07-06ALVES, Thayana da Conceição. Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN. 2018. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10412.https://repositorio.ufscar.br/handle/ufscar/10412Acai is a widely consumed fruit in the North Region of Brazil and has gained consumers in other regions of the country and abroad. With the increasing acai pulp demand, quality control measures become necessary to improve its trading; however, there are some problems, such as the fast degradation of the pulp, microbiological contamination and no knowledge on the behavior of the organic compounds present in the pulp of fruits of different origins, growing, seasonality, transport and processing. This study describes the influence of seasonality, growing conditions and genotypic variations on the acai pulp from Belém - PA by 1H NMR combined with chemometric methods, and structural characterization of the chemical constituents by LC-DAD-SPE/NMR. This work was performed in 4 stages: I) Identification of the greatest number of organic compounds by 1D and 2D NMR, without the need for isolation; II) Attainment of the chemical profile by 1H NMR combined with the chemometric treatment of the pulp of the fruits of 31 genotypes cultivated under agronomic control (Embrapa Amazônia Oriental) and also of commercial samples (Belém-PA); III) Verification of the correlation between the 1H NMR chemical profile and the physical-chemical data measured in the same samples; and IV) Identification of the organic compounds present in the commercial acai pulp extracts obtained with an ASETM (accelerated solvent extractor), being the major compounds obtained by 1D and 2D NMR, and the minor ones by LC-DAD-SPE/NMR with time-slice as trapping mode. Tendencies in the distribution of the acai pulp samples were observed according to the type of growing (agronomic control x without control), seasonality (harvest season x inter-harvest season), genetic improvement, and the storage system used by the retailers from Belém, and the compounds responsible for such tendencies were identified. The great variability in the physical-chemical data of the evaluated pulps was verified and, thus, there was no correlation with the 1H NMR spectral data. The ASE provided the best extracts when compared to extracts obtained with the conventional method. Some aromatic compounds were isolated from the acai pulp methanolic extract by LC-DAD-SPE, and their structures were determined based on the analysis of 1D and 2D NMR, UV and MS experiments. This study showed the potential of the high-resolution NMR technique to obtain chemical information from the lyophilized acai pulp. The traditional analysis methods (physical-chemical ones) were not viable, since they did not provide good comprehension of the variations of the acai pulps. The ASE extractor was a good alternative to perform the clean-up and extraction of the organic compounds present in acai and the time-slice mode proved efficient in the isolation of compounds at low concentration present in the acai pulp methanolic extract.O açaí é um alimento amplamente consumido em toda a Região Norte do Brasil e têm conquistado consumidores em outras regiões do país e no exterior. Com a crescente procura pela polpa, medidas de controle de qualidade se tornam necessárias para o auxílio da sua comercialização, mas existem alguns problemas como a rápida degradação da polpa, contaminação microbiológica e, nenhum conhecimento sobre o comportamento dos compostos orgânicos presentes na polpa dos frutos com diversas origens, cultivo, sazonalidade, transporte, processamento. No presente trabalho analisou-se a influência da sazonalidade, condições de cultivo, variações genotípicas da polpa do açaí de Belém - PA por RMN de 1H aliada a métodos quimiométricos e, a caracterização estrutural dos constituintes químicos em baixa concentração por LCDAD-SPE/NMR. A realização deste trabalho foi em 4 etapas: I) Identificação do maior número de compostos orgânicos através da RMN 1D e 2D, sem a necessidade de isolamento; II) Obtenção do perfil químico por RMN de 1H aliado a tratamentos quimiométricos das polpas dos frutos de 31 genótipos cultivados em condições de controle agronômico (Embrapa Amazônia Oriental) e também de amostras comerciais (Belém-PA); III) Verificação da correlação entre o perfil químico por RMN de 1H e os dados físico-químicos medidos nas mesmas amostras; e IV) Identificação dos compostos orgânicos presente nos extratos da polpa do açaí comercial obtidos com o ASETM (extração acelerada por solvente), sendo os majoritários por RMN 1D e 2D e, os minoritários utilizando LC-DAD-SPE/NMR com time-slice como modo de trapeamento. Foram verificadas tendências na distribuição das amostras das polpas do açaí de acordo com o tipo de cultivo (controle agronômico x sem controle), a sazonalidade (safra x entressafra), melhoramento genético e o modo de armazenamento realizado pelos comerciantes de Belém e quais os compostos responsáveis por essas observações. Foi verificada a grande variabilidade nos dados físico-químicos das polpas avaliadas e, dessa forma não houve correlação com os dados espectrais por RMN de 1H. O uso do ASE forneceu melhores extratos quando comparados a extratos obtidos por método de extração convencional e, da fração metanólica da polpa de açaí foram isolados alguns compostos aromáticos por LCDAD-SPE que tiveram suas estruturas identificadas com base na análise dos experimentos de RMN 1D e 2D, UV e EM. Esse trabalho mostrou o potencial da técnica de RMN de alta resolução na obtenção de informações químicas das polpas do açaí liofilizadas. Os métodos tradicionais de análises (físico-químicos) não se mostraram viáveis pois não forneceram boa compreensão sobre as variações das polpas do açaí. O extrator acelerado por solvente foi uma boa alternativa para realização de clean-up e extração de compostos orgânicos presentes no açaí e o modo time-slice mostrou-se eficiente para o isolamento de compostos em pequena concentração presente no extrato metanólico da polpa do açaí.Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)142102/2014-8porUniversidade Federal de São CarlosCâmpus São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarEuterpe oleraceaAçaíRessonância magnética nuclearFingerprintLC-DAD-SPE/NMRCIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ORGANICAPerfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMNFingerprint profile and structural characterization of the metabolites in açaí berry pulp (Euterpe oleracea Mart.) by NMRinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisOnlineinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARLICENSElicense.txtlicense.txttext/plain; charset=utf-81957https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10412/5/license.txtae0398b6f8b235e40ad82cba6c50031dMD55ORIGINALALVES_Thayana_2018.pdfALVES_Thayana_2018.pdfapplication/pdf10427223https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10412/6/ALVES_Thayana_2018.pdfb29693fa405e699c88330c773e25e28fMD56THUMBNAILALVES_Thayana_2018.pdf.jpgALVES_Thayana_2018.pdf.jpgIM Thumbnailimage/jpeg10540https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10412/7/ALVES_Thayana_2018.pdf.jpga5064e29e3e10a20b44165cde820b6cbMD57ufscar/104122019-09-11 03:48:30.295oai:repositorio.ufscar.br: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Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-05-25T12:56:22.481851Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false |
dc.title.por.fl_str_mv |
Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN |
dc.title.alternative.eng.fl_str_mv |
Fingerprint profile and structural characterization of the metabolites in açaí berry pulp (Euterpe oleracea Mart.) by NMR |
title |
Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN |
spellingShingle |
Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN Alves, Thayana da Conceição Euterpe oleracea Açaí Ressonância magnética nuclear Fingerprint LC-DAD-SPE/NMR CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ORGANICA |
title_short |
Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN |
title_full |
Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN |
title_fullStr |
Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN |
title_full_unstemmed |
Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN |
title_sort |
Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN |
author |
Alves, Thayana da Conceição |
author_facet |
Alves, Thayana da Conceição |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/0399434594190877 |
dc.contributor.author.fl_str_mv |
Alves, Thayana da Conceição |
dc.contributor.advisor1.fl_str_mv |
Ferreira, Antonio Gilberto |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/3676462220401452 |
contributor_str_mv |
Ferreira, Antonio Gilberto |
dc.subject.por.fl_str_mv |
Euterpe oleracea Açaí Ressonância magnética nuclear |
topic |
Euterpe oleracea Açaí Ressonância magnética nuclear Fingerprint LC-DAD-SPE/NMR CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ORGANICA |
dc.subject.eng.fl_str_mv |
Fingerprint LC-DAD-SPE/NMR |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ORGANICA |
description |
Acai is a widely consumed fruit in the North Region of Brazil and has gained consumers in other regions of the country and abroad. With the increasing acai pulp demand, quality control measures become necessary to improve its trading; however, there are some problems, such as the fast degradation of the pulp, microbiological contamination and no knowledge on the behavior of the organic compounds present in the pulp of fruits of different origins, growing, seasonality, transport and processing. This study describes the influence of seasonality, growing conditions and genotypic variations on the acai pulp from Belém - PA by 1H NMR combined with chemometric methods, and structural characterization of the chemical constituents by LC-DAD-SPE/NMR. This work was performed in 4 stages: I) Identification of the greatest number of organic compounds by 1D and 2D NMR, without the need for isolation; II) Attainment of the chemical profile by 1H NMR combined with the chemometric treatment of the pulp of the fruits of 31 genotypes cultivated under agronomic control (Embrapa Amazônia Oriental) and also of commercial samples (Belém-PA); III) Verification of the correlation between the 1H NMR chemical profile and the physical-chemical data measured in the same samples; and IV) Identification of the organic compounds present in the commercial acai pulp extracts obtained with an ASETM (accelerated solvent extractor), being the major compounds obtained by 1D and 2D NMR, and the minor ones by LC-DAD-SPE/NMR with time-slice as trapping mode. Tendencies in the distribution of the acai pulp samples were observed according to the type of growing (agronomic control x without control), seasonality (harvest season x inter-harvest season), genetic improvement, and the storage system used by the retailers from Belém, and the compounds responsible for such tendencies were identified. The great variability in the physical-chemical data of the evaluated pulps was verified and, thus, there was no correlation with the 1H NMR spectral data. The ASE provided the best extracts when compared to extracts obtained with the conventional method. Some aromatic compounds were isolated from the acai pulp methanolic extract by LC-DAD-SPE, and their structures were determined based on the analysis of 1D and 2D NMR, UV and MS experiments. This study showed the potential of the high-resolution NMR technique to obtain chemical information from the lyophilized acai pulp. The traditional analysis methods (physical-chemical ones) were not viable, since they did not provide good comprehension of the variations of the acai pulps. The ASE extractor was a good alternative to perform the clean-up and extraction of the organic compounds present in acai and the time-slice mode proved efficient in the isolation of compounds at low concentration present in the acai pulp methanolic extract. |
publishDate |
2018 |
dc.date.accessioned.fl_str_mv |
2018-08-29T13:35:27Z |
dc.date.available.fl_str_mv |
2018-08-29T13:35:27Z |
dc.date.issued.fl_str_mv |
2018-07-06 |
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.citation.fl_str_mv |
ALVES, Thayana da Conceição. Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN. 2018. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10412. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/10412 |
identifier_str_mv |
ALVES, Thayana da Conceição. Perfil químico e caracterização estrutural de metabólitos na polpa do açaí (Euterpe oleracea Mart.) por RMN. 2018. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10412. |
url |
https://repositorio.ufscar.br/handle/ufscar/10412 |
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por |
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openAccess |
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Universidade Federal de São Carlos Câmpus São Carlos |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química - PPGQ |
dc.publisher.initials.fl_str_mv |
UFSCar |
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Universidade Federal de São Carlos Câmpus São Carlos |
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