Fenilpropanoides da Paspalum atratum

Detalhes bibliográficos
Autor(a) principal: Pinto, Luciano da Silva [UNESP]
Data de Publicação: 2015
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Repositório Institucional da UNESP
Texto Completo: http://hdl.handle.net/11449/124482
Resumo: This work describes the phytochemical study on ethanol extract from aerial parts of Paspalum atratum Swalen (Poaceae). The Paspalum genus is one of the most important grasses in Brazil and has characteristics compatible with its utilization in pastures for cattle. Phenylpropanoids were isolated by chromatographic methods (CC and HPLC) for the first time in this genus. These phenylpropanoids were identified as (R)-rosmarinic acid (RA, 1), 3-O-caffeoylquinic acid (2), phenylalanine (3), cis- and trans-3-O-coumaroylquinic acids (4 and 5), 5-O-caffeoylquinic acid (6, chlorogenic acid), 4-O-caffeoylquinic acid (7), and caffeic acid (8) by analyses of their MS, 1H and 13C NMR data, including COSY, HMBC, HSQC and DOSY, and comparison of these data with those reported in the literature for these type of compounds. The major compound isolated from the ethanol extract was RA (4.4%). It was used as standard for qualitative and quantitative analyses of extract. An efficient HPLC-DAD method for determination of RA in extract was established (r2 = 0.9979). The limit of detection (LOD) and limit of quantification (LOQ) were 4.00 and 12.13 μg/mL, respectively, and the validated range was 12.1-100.0 μg/mL. The intra-day and inter-day precisions of the method were evaluated by analyzing the blank solution spiked by RA. The standard deviation (SD) as evaluation parameter for the intra-day precision of peak area of target analyte was in the range of 1.57-2.06%. The inter-day precision (7 days) of the method was in the range of 0.54-1.69%. Satisfactory recovery (75-78%), evaluated by standard additions method, was achieved.
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spelling Fenilpropanoides da Paspalum atratumGramíneaRessonancia magnetica nuclearAnalise de varianciaPastagensCromatografia líquida de alta eficiênciaFenilalaninaThis work describes the phytochemical study on ethanol extract from aerial parts of Paspalum atratum Swalen (Poaceae). The Paspalum genus is one of the most important grasses in Brazil and has characteristics compatible with its utilization in pastures for cattle. Phenylpropanoids were isolated by chromatographic methods (CC and HPLC) for the first time in this genus. These phenylpropanoids were identified as (R)-rosmarinic acid (RA, 1), 3-O-caffeoylquinic acid (2), phenylalanine (3), cis- and trans-3-O-coumaroylquinic acids (4 and 5), 5-O-caffeoylquinic acid (6, chlorogenic acid), 4-O-caffeoylquinic acid (7), and caffeic acid (8) by analyses of their MS, 1H and 13C NMR data, including COSY, HMBC, HSQC and DOSY, and comparison of these data with those reported in the literature for these type of compounds. The major compound isolated from the ethanol extract was RA (4.4%). It was used as standard for qualitative and quantitative analyses of extract. An efficient HPLC-DAD method for determination of RA in extract was established (r2 = 0.9979). The limit of detection (LOD) and limit of quantification (LOQ) were 4.00 and 12.13 μg/mL, respectively, and the validated range was 12.1-100.0 μg/mL. The intra-day and inter-day precisions of the method were evaluated by analyzing the blank solution spiked by RA. The standard deviation (SD) as evaluation parameter for the intra-day precision of peak area of target analyte was in the range of 1.57-2.06%. The inter-day precision (7 days) of the method was in the range of 0.54-1.69%. Satisfactory recovery (75-78%), evaluated by standard additions method, was achieved.Este trabalho descreve o estudo fitoquímico do extrato etanólico de Paspalum atratum Swalen (Poaceae). O gênero Paspalum é o mais importante das gramíneas no Brasil e possui características compatíveis com a utilização no pastejo. Fenilpropanoides foram isolados por métodos cromatográficos (CC, CLAE) pela primeira vez neste gênero. Estes fenilpropanoides foram identificados como: (R)-ácido rosmarínico, (AR, 1), ácido 3-O-cafeoilquínico (2), fenilalanina (3), ácidos cis- e trans-coumaroilquínico (4 e 5), ácido 5-O-cafeoilquínico (6), ácido 4-O-cafeoilquínico (7) e ácido cafeico (8) pela análise de seus dados de EM, RMN de 1H e de 13C, incluindo COSY, HMBC, HSQC, TOCSY-1D e DOSY, e pela comparação destes dados com aqueles descritos na literatura para estas substâncias. A substância majoritária no extrato etanólico foi o AR (4,4%). Esta foi usada como padrão em análises qualitativas e quantitativas do extrato. Um método eficiente em CLAE-DAD para determinação de AR no extrato foi estabelecido (r2 = 0,9979). O limite de detecção (LD) e limite de quantificação (LQ) foram 4,00 e 12,13 μg/mL respectivamente, e a faixa de linearidade foi 12,1-100,0 μg/mL. As precisões intradia e interdia do método foram avaliadas pela análise das soluções de padrão AR. O desvio padrão da área do pico do analito foi utilizado como parâmetro de avaliação da precisão intradia, compreendendo o intervalo de 1,57-2,06%. A precisão interdia (7 dias) do método compreendeu o intervalo de 0,54-1,69%. A recuperação, avaliada pela adição do padrão AR, foi satisfatória (75-78%.Universidade Estadual Paulista (Unesp)Lopes, Lucia Maria Xavier [UNESP]Nascimento, Isabele Rodrigues [UNESP]Universidade Estadual Paulista (Unesp)Pinto, Luciano da Silva [UNESP]2015-07-13T12:10:22Z2015-07-13T12:10:22Z2015-02-24info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesis84 f. : il.application/pdfPINTO, Luciano da Silva. Fenilpropanoides da Paspalum atratum. 2015. 84 f. Dissertação (mestrado) - Universidade Estadual Paulista Júlio de Mesquita Filho, Instituto de Quimica., 2015.http://hdl.handle.net/11449/124482000827283000827283.pdf33004030072P859813534420370510124211071790021Alephreponame:Repositório Institucional da UNESPinstname:Universidade Estadual Paulista (UNESP)instacron:UNESPporinfo:eu-repo/semantics/openAccess2023-10-05T06:07:37Zoai:repositorio.unesp.br:11449/124482Repositório InstitucionalPUBhttp://repositorio.unesp.br/oai/requestopendoar:29462024-08-05T14:06:03.746356Repositório Institucional da UNESP - Universidade Estadual Paulista (UNESP)false
dc.title.none.fl_str_mv Fenilpropanoides da Paspalum atratum
title Fenilpropanoides da Paspalum atratum
spellingShingle Fenilpropanoides da Paspalum atratum
Pinto, Luciano da Silva [UNESP]
Gramínea
Ressonancia magnetica nuclear
Analise de variancia
Pastagens
Cromatografia líquida de alta eficiência
Fenilalanina
title_short Fenilpropanoides da Paspalum atratum
title_full Fenilpropanoides da Paspalum atratum
title_fullStr Fenilpropanoides da Paspalum atratum
title_full_unstemmed Fenilpropanoides da Paspalum atratum
title_sort Fenilpropanoides da Paspalum atratum
author Pinto, Luciano da Silva [UNESP]
author_facet Pinto, Luciano da Silva [UNESP]
author_role author
dc.contributor.none.fl_str_mv Lopes, Lucia Maria Xavier [UNESP]
Nascimento, Isabele Rodrigues [UNESP]
Universidade Estadual Paulista (Unesp)
dc.contributor.author.fl_str_mv Pinto, Luciano da Silva [UNESP]
dc.subject.por.fl_str_mv Gramínea
Ressonancia magnetica nuclear
Analise de variancia
Pastagens
Cromatografia líquida de alta eficiência
Fenilalanina
topic Gramínea
Ressonancia magnetica nuclear
Analise de variancia
Pastagens
Cromatografia líquida de alta eficiência
Fenilalanina
description This work describes the phytochemical study on ethanol extract from aerial parts of Paspalum atratum Swalen (Poaceae). The Paspalum genus is one of the most important grasses in Brazil and has characteristics compatible with its utilization in pastures for cattle. Phenylpropanoids were isolated by chromatographic methods (CC and HPLC) for the first time in this genus. These phenylpropanoids were identified as (R)-rosmarinic acid (RA, 1), 3-O-caffeoylquinic acid (2), phenylalanine (3), cis- and trans-3-O-coumaroylquinic acids (4 and 5), 5-O-caffeoylquinic acid (6, chlorogenic acid), 4-O-caffeoylquinic acid (7), and caffeic acid (8) by analyses of their MS, 1H and 13C NMR data, including COSY, HMBC, HSQC and DOSY, and comparison of these data with those reported in the literature for these type of compounds. The major compound isolated from the ethanol extract was RA (4.4%). It was used as standard for qualitative and quantitative analyses of extract. An efficient HPLC-DAD method for determination of RA in extract was established (r2 = 0.9979). The limit of detection (LOD) and limit of quantification (LOQ) were 4.00 and 12.13 μg/mL, respectively, and the validated range was 12.1-100.0 μg/mL. The intra-day and inter-day precisions of the method were evaluated by analyzing the blank solution spiked by RA. The standard deviation (SD) as evaluation parameter for the intra-day precision of peak area of target analyte was in the range of 1.57-2.06%. The inter-day precision (7 days) of the method was in the range of 0.54-1.69%. Satisfactory recovery (75-78%), evaluated by standard additions method, was achieved.
publishDate 2015
dc.date.none.fl_str_mv 2015-07-13T12:10:22Z
2015-07-13T12:10:22Z
2015-02-24
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
format masterThesis
status_str publishedVersion
dc.identifier.uri.fl_str_mv PINTO, Luciano da Silva. Fenilpropanoides da Paspalum atratum. 2015. 84 f. Dissertação (mestrado) - Universidade Estadual Paulista Júlio de Mesquita Filho, Instituto de Quimica., 2015.
http://hdl.handle.net/11449/124482
000827283
000827283.pdf
33004030072P8
5981353442037051
0124211071790021
identifier_str_mv PINTO, Luciano da Silva. Fenilpropanoides da Paspalum atratum. 2015. 84 f. Dissertação (mestrado) - Universidade Estadual Paulista Júlio de Mesquita Filho, Instituto de Quimica., 2015.
000827283
000827283.pdf
33004030072P8
5981353442037051
0124211071790021
url http://hdl.handle.net/11449/124482
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 84 f. : il.
application/pdf
dc.publisher.none.fl_str_mv Universidade Estadual Paulista (Unesp)
publisher.none.fl_str_mv Universidade Estadual Paulista (Unesp)
dc.source.none.fl_str_mv Aleph
reponame:Repositório Institucional da UNESP
instname:Universidade Estadual Paulista (UNESP)
instacron:UNESP
instname_str Universidade Estadual Paulista (UNESP)
instacron_str UNESP
institution UNESP
reponame_str Repositório Institucional da UNESP
collection Repositório Institucional da UNESP
repository.name.fl_str_mv Repositório Institucional da UNESP - Universidade Estadual Paulista (UNESP)
repository.mail.fl_str_mv
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