Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto
Autor(a) principal: | |
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Data de Publicação: | 2009 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFRN |
Texto Completo: | https://repositorio.ufrn.br/jspui/handle/123456789/15887 |
Resumo: | The aim of the present study was to extract vegetable oil from brown linseed (Linum usitatissimum L.), determine fatty acid levels, the antioxidant capacity of the extracted oil and perform a rapid economic assessment of the SFE process in the manufacture of oil. The experiments were conducted in a test bench extractor capable of operating with carbon dioxide and co-solvents, obeying 23 factorial planning with central point in triplicate, and having process yield as response variable and pressure, temperature and percentage of cosolvent as independent variables. The yield (mass of extracted oil/mass of raw material used) ranged from 2.2% to 28.8%, with the best results obtained at 250 bar and 50ºC, using 5% (v/v) ethanol co-solvent. The influence of the variables on extraction kinetics and on the composition of the linseed oil obtained was investigated. The extraction kinetic curves obtained were based on different mathematical models available in the literature. The Martínez et al. (2003) model and the Simple Single Plate (SSP) model discussed by Gaspar et al. (2003) represented the experimental data with the lowest mean square errors (MSE). A manufacturing cost of US$17.85/kgoil was estimated for the production of linseed oil using TECANALYSIS software and the Rosa and Meireles method (2005). To establish comparisons with SFE, conventional extraction tests were conducted with a Soxhlet device using petroleum ether. These tests obtained mean yields of 35.2% for an extraction time of 5h. All the oil samples were sterilized and characterized in terms of their composition in fatty acids (FA) using gas chromatography. The main fatty acids detected were: palmitic (C16:0), stearic (C18:0), oleic (C18:1), linoleic (C18:2n-6) and α-linolenic (C18:3n-3). The FA contents obtained with Soxhlet dif ered from those obtained with SFE, with higher percentages of saturated and monounsaturated FA with the Soxhlet technique using petroleum ether. With respect to α-linolenic content (main component of linseed oil) in the samples, SFE performed better than Soxhlet extraction, obtaining percentages between 51.18% and 52.71%, whereas with Soxhlet extraction it was 47.84%. The antioxidant activity of the oil was assessed in the β-carotene/linoleic acid system. The percentages of inhibition of the oxidative process reached 22.11% for the SFE oil, but only 6.09% for commercial oil (cold pressing), suggesting that the SFE technique better preserves the phenolic compounds present in the seed, which are likely responsible for the antioxidant nature of the oil. In vitro tests with the sample displaying the best antioxidant response were conducted in rat liver homogenate to investigate the inhibition of spontaneous lipid peroxidation or autooxidation of biological tissue. Linseed oil proved to be more efficient than fish oil (used as standard) in decreasing lipid peroxidation in the liver tissue of Wistar rats, yielding similar results to those obtained with the use of BHT (synthetic antioxidant). Inhibitory capacity may be explained by the presence of phenolic compounds with antioxidant activity in the linseed oil. The results obtained indicate the need for more detailed studies, given the importance of linseed oil as one of the greatest sources of ω3 among vegetable oils |
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Galvão, Elisângela Lopeshttp://lattes.cnpq.br/4522095618671600http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4787769D1Moreira, Ana Vladia Bandeirahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4799337D6Cardozo Filho, Lúciohttp://lattes.cnpq.br/2710474728753403Oliveira, Humberto Neves Maia dehttp://lattes.cnpq.br/7302633941782540Chiavone Filho, Osvaldohttp://lattes.cnpq.br/2621516646153655Souza, Carlson Pereira dehttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781094H3Sousa, Elisa Maria Bittencourt Dutra de2014-12-17T15:01:47Z2009-12-032014-12-17T15:01:47Z2009-05-15GALVÃO, Elisângela Lopes. Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto. 2009. 159 f. Tese (Doutorado em Pesquisa e Desenvolvimento de Tecnologias Regionais) - Universidade Federal do Rio Grande do Norte, Natal, 2009.https://repositorio.ufrn.br/jspui/handle/123456789/15887The aim of the present study was to extract vegetable oil from brown linseed (Linum usitatissimum L.), determine fatty acid levels, the antioxidant capacity of the extracted oil and perform a rapid economic assessment of the SFE process in the manufacture of oil. The experiments were conducted in a test bench extractor capable of operating with carbon dioxide and co-solvents, obeying 23 factorial planning with central point in triplicate, and having process yield as response variable and pressure, temperature and percentage of cosolvent as independent variables. The yield (mass of extracted oil/mass of raw material used) ranged from 2.2% to 28.8%, with the best results obtained at 250 bar and 50ºC, using 5% (v/v) ethanol co-solvent. The influence of the variables on extraction kinetics and on the composition of the linseed oil obtained was investigated. The extraction kinetic curves obtained were based on different mathematical models available in the literature. The Martínez et al. (2003) model and the Simple Single Plate (SSP) model discussed by Gaspar et al. (2003) represented the experimental data with the lowest mean square errors (MSE). A manufacturing cost of US$17.85/kgoil was estimated for the production of linseed oil using TECANALYSIS software and the Rosa and Meireles method (2005). To establish comparisons with SFE, conventional extraction tests were conducted with a Soxhlet device using petroleum ether. These tests obtained mean yields of 35.2% for an extraction time of 5h. All the oil samples were sterilized and characterized in terms of their composition in fatty acids (FA) using gas chromatography. The main fatty acids detected were: palmitic (C16:0), stearic (C18:0), oleic (C18:1), linoleic (C18:2n-6) and α-linolenic (C18:3n-3). The FA contents obtained with Soxhlet dif ered from those obtained with SFE, with higher percentages of saturated and monounsaturated FA with the Soxhlet technique using petroleum ether. With respect to α-linolenic content (main component of linseed oil) in the samples, SFE performed better than Soxhlet extraction, obtaining percentages between 51.18% and 52.71%, whereas with Soxhlet extraction it was 47.84%. The antioxidant activity of the oil was assessed in the β-carotene/linoleic acid system. The percentages of inhibition of the oxidative process reached 22.11% for the SFE oil, but only 6.09% for commercial oil (cold pressing), suggesting that the SFE technique better preserves the phenolic compounds present in the seed, which are likely responsible for the antioxidant nature of the oil. In vitro tests with the sample displaying the best antioxidant response were conducted in rat liver homogenate to investigate the inhibition of spontaneous lipid peroxidation or autooxidation of biological tissue. Linseed oil proved to be more efficient than fish oil (used as standard) in decreasing lipid peroxidation in the liver tissue of Wistar rats, yielding similar results to those obtained with the use of BHT (synthetic antioxidant). Inhibitory capacity may be explained by the presence of phenolic compounds with antioxidant activity in the linseed oil. The results obtained indicate the need for more detailed studies, given the importance of linseed oil as one of the greatest sources of ω3 among vegetable oilsO presente trabalho teve como objetivo geral extrair o óleo vegetal da linhaça (Linum usitatissimum L.) da variedade marrom fazendo uso de dióxido de carbono em condições supercríticas e de solvente orgânico, avaliar os teores de ácidos graxos e a capacidade antioxidante do óleo extraído e ainda realizar a avaliação econômica rápida do processo EFS de manufatura do óleo. Os experimentos foram conduzidos em um extrator de bancada, capaz de operar com dióxido de carbono e co-solventes, obedecendo a um planejamento fatorial 2³ com triplicata no ponto central, tendo como variável resposta o rendimento do processo e como variáveis independentes a pressão, a temperatura e o percentual de co-solvente. Os rendimentos (massa de óleo extraído/ massa de matéria-prima utilizada) variaram de 2,2 a 28,8%, tendo os melhores resultados sido obtidos a 250 bar e 50°C, com uso do co-solvente etanol a 5% (v/v). A influência das variáveis sobre a cinética de extração e sobre a composição do óleo de linhaça obtido também foi investigada. As curvas cinéticas de extração obtidas foram modeladas por diferentes modelos matemáticos disponíveis na literatura. Os modelos de Martínez et al. (2003) e o Simple Single Plate (SSP) de Gaspar et al. (2003) representaram os dados experimentais com os menores erros quadráticos médios (MSE). O custo de manufatura de 17,85 US$/kgóleo foi estimado para produção do óleo de linhaça utilizando o software TECANALYSIS e a metodologia de Rosa e Meireles (2005). Com o intuito de estabelecer comparações com a EFS, foram realizados ensaios de extração por técnica convencional em aparato Soxhlet utilizando éter de petróleo. Estes apresentaram rendimentos médios de 35,2 % para um tempo de extração de 5h. Todas as amostras de óleo obtidas foram esterificadas e caracterizadas em termos de sua composição em ácidos graxos (AGs) usando a cromatografia gasosa. Os principais ácidos graxos detectados foram: palmítico (C16:0), esteárico (C18:0), oléico (C18:1), linoléico (C18:2n-6) e α-linolênico (C18:3n-3). Os teores dos AGs obtidos com Soxhlet diferiram daqueles obtidos para a EFS, com percentuais de AGs saturados e monoinsaturados mais elevados para a técnica Soxhlet com éter de petróleo. Com relação ao teor do ácido α-linolênico (componente majoritário do óleo de linhaça) nas amostras, a EFS se mostrou mais vantajosa que a extração Soxhlet, apresentando percentuais de 51,18 a 52,71%, enquanto que na extração Soxhlet, este foi de 47,84%. A atividade antioxidante do óleo foi avaliada no sistema de co-oxidação b-caroteno/ácido linoléico. Os percentuais de inibição do processo oxidativo chegaram a 22,11% para o óleo da EFS, sendo de apenas 6,09% para o óleo comercial extraído a frio, o que sugere que a técnica EFS preserva melhor os compostos fenólicos presentes na semente, compostos estes, provavelmente responsáveis pelo caráter antioxidante do óleo. Testes in vitro com a amostra de melhor resposta antioxidante foram realizados em homogenato de fígado de ratos, de forma a investigar a inibição da peroxidação lipídica espontânea ou autoxidação do tecido biológico. O óleo de linhaça se mostrou mais eficiente que o óleo de peixe (usado como padrão) na diminuição da peroxidação lipídica do tecido hepático dos ratos Wistar, apresentando resultados equivalentes aos obtidos com o uso do BHT (antioxidante sintético). A capacidade inibitória pode ser atribuída à presença de compostos fenólicos com atividade antioxidante presentes no óleo de linhaça. Os resultados obtidos indicam a necessidade de estudos mais aprofundados tendo em vista a importância do óleo de linhaça como uma das maiores fontes de ω3 dentre os óleos vegetaisConselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal do Rio Grande do NortePrograma de Pós-Graduação em Engenharia QuímicaUFRNBRPesquisa e Desenvolvimento de Tecnologias RegionaisExtração supercríticaDióxido de carbonoÓleo de linhaçaLinum usitatissimum L.Atividade antioxidanteSupercritical extractionCarbon dioxideLinseed oilLinum usitatissimum LAntioxidant activityCNPQ::ENGENHARIAS::ENGENHARIA QUIMICAExtração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produtoinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFRNinstname:Universidade Federal do Rio Grande do Norte (UFRN)instacron:UFRNORIGINALElisangelaLG.pdfapplication/pdf1590433https://repositorio.ufrn.br/bitstream/123456789/15887/1/ElisangelaLG.pdf344724364926bacba0bb6a0d130edd0dMD51TEXTElisangelaLG.pdf.txtElisangelaLG.pdf.txtExtracted texttext/plain274996https://repositorio.ufrn.br/bitstream/123456789/15887/6/ElisangelaLG.pdf.txt2e53111b0ea12ec2c5099c8ebd4275ffMD56THUMBNAILElisangelaLG.pdf.jpgElisangelaLG.pdf.jpgIM Thumbnailimage/jpeg4566https://repositorio.ufrn.br/bitstream/123456789/15887/7/ElisangelaLG.pdf.jpg3e5dc8800f8755af97c348696e4a035cMD57123456789/158872017-11-02 05:16:11.9oai:https://repositorio.ufrn.br:123456789/15887Repositório de PublicaçõesPUBhttp://repositorio.ufrn.br/oai/opendoar:2017-11-02T08:16:11Repositório Institucional da UFRN - Universidade Federal do Rio Grande do Norte (UFRN)false |
dc.title.por.fl_str_mv |
Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto |
title |
Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto |
spellingShingle |
Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto Galvão, Elisângela Lopes Extração supercrítica Dióxido de carbono Óleo de linhaça Linum usitatissimum L. Atividade antioxidante Supercritical extraction Carbon dioxide Linseed oil Linum usitatissimum L Antioxidant activity CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA |
title_short |
Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto |
title_full |
Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto |
title_fullStr |
Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto |
title_full_unstemmed |
Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto |
title_sort |
Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto |
author |
Galvão, Elisângela Lopes |
author_facet |
Galvão, Elisângela Lopes |
author_role |
author |
dc.contributor.authorID.por.fl_str_mv |
|
dc.contributor.authorLattes.por.fl_str_mv |
http://lattes.cnpq.br/4522095618671600 |
dc.contributor.advisorID.por.fl_str_mv |
|
dc.contributor.advisorLattes.por.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4787769D1 |
dc.contributor.advisor-co1ID.por.fl_str_mv |
|
dc.contributor.referees1.pt_BR.fl_str_mv |
Cardozo Filho, Lúcio |
dc.contributor.referees1ID.por.fl_str_mv |
|
dc.contributor.referees1Lattes.por.fl_str_mv |
http://lattes.cnpq.br/2710474728753403 |
dc.contributor.referees2.pt_BR.fl_str_mv |
Oliveira, Humberto Neves Maia de |
dc.contributor.referees2ID.por.fl_str_mv |
|
dc.contributor.referees2Lattes.por.fl_str_mv |
http://lattes.cnpq.br/7302633941782540 |
dc.contributor.referees3.pt_BR.fl_str_mv |
Chiavone Filho, Osvaldo |
dc.contributor.referees3ID.por.fl_str_mv |
|
dc.contributor.referees3Lattes.por.fl_str_mv |
http://lattes.cnpq.br/2621516646153655 |
dc.contributor.referees4.pt_BR.fl_str_mv |
Souza, Carlson Pereira de |
dc.contributor.referees4ID.por.fl_str_mv |
|
dc.contributor.referees4Lattes.por.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781094H3 |
dc.contributor.author.fl_str_mv |
Galvão, Elisângela Lopes |
dc.contributor.advisor-co1.fl_str_mv |
Moreira, Ana Vladia Bandeira |
dc.contributor.advisor-co1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4799337D6 |
dc.contributor.advisor1.fl_str_mv |
Sousa, Elisa Maria Bittencourt Dutra de |
contributor_str_mv |
Moreira, Ana Vladia Bandeira Sousa, Elisa Maria Bittencourt Dutra de |
dc.subject.por.fl_str_mv |
Extração supercrítica Dióxido de carbono Óleo de linhaça Linum usitatissimum L. Atividade antioxidante |
topic |
Extração supercrítica Dióxido de carbono Óleo de linhaça Linum usitatissimum L. Atividade antioxidante Supercritical extraction Carbon dioxide Linseed oil Linum usitatissimum L Antioxidant activity CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA |
dc.subject.eng.fl_str_mv |
Supercritical extraction Carbon dioxide Linseed oil Linum usitatissimum L Antioxidant activity |
dc.subject.cnpq.fl_str_mv |
CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA |
description |
The aim of the present study was to extract vegetable oil from brown linseed (Linum usitatissimum L.), determine fatty acid levels, the antioxidant capacity of the extracted oil and perform a rapid economic assessment of the SFE process in the manufacture of oil. The experiments were conducted in a test bench extractor capable of operating with carbon dioxide and co-solvents, obeying 23 factorial planning with central point in triplicate, and having process yield as response variable and pressure, temperature and percentage of cosolvent as independent variables. The yield (mass of extracted oil/mass of raw material used) ranged from 2.2% to 28.8%, with the best results obtained at 250 bar and 50ºC, using 5% (v/v) ethanol co-solvent. The influence of the variables on extraction kinetics and on the composition of the linseed oil obtained was investigated. The extraction kinetic curves obtained were based on different mathematical models available in the literature. The Martínez et al. (2003) model and the Simple Single Plate (SSP) model discussed by Gaspar et al. (2003) represented the experimental data with the lowest mean square errors (MSE). A manufacturing cost of US$17.85/kgoil was estimated for the production of linseed oil using TECANALYSIS software and the Rosa and Meireles method (2005). To establish comparisons with SFE, conventional extraction tests were conducted with a Soxhlet device using petroleum ether. These tests obtained mean yields of 35.2% for an extraction time of 5h. All the oil samples were sterilized and characterized in terms of their composition in fatty acids (FA) using gas chromatography. The main fatty acids detected were: palmitic (C16:0), stearic (C18:0), oleic (C18:1), linoleic (C18:2n-6) and α-linolenic (C18:3n-3). The FA contents obtained with Soxhlet dif ered from those obtained with SFE, with higher percentages of saturated and monounsaturated FA with the Soxhlet technique using petroleum ether. With respect to α-linolenic content (main component of linseed oil) in the samples, SFE performed better than Soxhlet extraction, obtaining percentages between 51.18% and 52.71%, whereas with Soxhlet extraction it was 47.84%. The antioxidant activity of the oil was assessed in the β-carotene/linoleic acid system. The percentages of inhibition of the oxidative process reached 22.11% for the SFE oil, but only 6.09% for commercial oil (cold pressing), suggesting that the SFE technique better preserves the phenolic compounds present in the seed, which are likely responsible for the antioxidant nature of the oil. In vitro tests with the sample displaying the best antioxidant response were conducted in rat liver homogenate to investigate the inhibition of spontaneous lipid peroxidation or autooxidation of biological tissue. Linseed oil proved to be more efficient than fish oil (used as standard) in decreasing lipid peroxidation in the liver tissue of Wistar rats, yielding similar results to those obtained with the use of BHT (synthetic antioxidant). Inhibitory capacity may be explained by the presence of phenolic compounds with antioxidant activity in the linseed oil. The results obtained indicate the need for more detailed studies, given the importance of linseed oil as one of the greatest sources of ω3 among vegetable oils |
publishDate |
2009 |
dc.date.available.fl_str_mv |
2009-12-03 2014-12-17T15:01:47Z |
dc.date.issued.fl_str_mv |
2009-05-15 |
dc.date.accessioned.fl_str_mv |
2014-12-17T15:01:47Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/doctoralThesis |
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dc.identifier.citation.fl_str_mv |
GALVÃO, Elisângela Lopes. Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto. 2009. 159 f. Tese (Doutorado em Pesquisa e Desenvolvimento de Tecnologias Regionais) - Universidade Federal do Rio Grande do Norte, Natal, 2009. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufrn.br/jspui/handle/123456789/15887 |
identifier_str_mv |
GALVÃO, Elisângela Lopes. Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto. 2009. 159 f. Tese (Doutorado em Pesquisa e Desenvolvimento de Tecnologias Regionais) - Universidade Federal do Rio Grande do Norte, Natal, 2009. |
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https://repositorio.ufrn.br/jspui/handle/123456789/15887 |
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Universidade Federal do Rio Grande do Norte |
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Programa de Pós-Graduação em Engenharia Química |
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UFRN |
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BR |
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Universidade Federal do Rio Grande do Norte |
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