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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

Extra??o supercr?tica do ?leo de linha?a: constru??o do extrator, estudo de par?metros de processo, avalia??o qu?mica e antioxidante do produto

Galv?o, Elis?ngela Lopes 15 May 2009 (has links)
Made available in DSpace on 2014-12-17T15:01:47Z (GMT). No. of bitstreams: 1 ElisangelaLG.pdf: 1590433 bytes, checksum: 344724364926bacba0bb6a0d130edd0d (MD5) Previous issue date: 2009-05-15 / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico / 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 50?C, 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 Mart?nez 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 / O presente trabalho teve como objetivo geral extrair o ?leo vegetal da linha?a (Linum usitatissimum L.) da variedade marrom fazendo uso de di?xido de carbono em condi??es supercr?ticas e de solvente org?nico, avaliar os teores de ?cidos graxos e a capacidade antioxidante do ?leo extra?do e ainda realizar a avalia??o econ?mica r?pida do processo EFS de manufatura do ?leo. Os experimentos foram conduzidos em um extrator de bancada, capaz de operar com di?xido de carbono e co-solventes, obedecendo a um planejamento fatorial 2? com triplicata no ponto central, tendo como vari?vel resposta o rendimento do processo e como vari?veis independentes a press?o, a temperatura e o percentual de co-solvente. Os rendimentos (massa de ?leo extra?do/ massa de mat?ria-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 influ?ncia das vari?veis sobre a cin?tica de extra??o e sobre a composi??o do ?leo de linha?a obtido tamb?m foi investigada. As curvas cin?ticas de extra??o obtidas foram modeladas por diferentes modelos matem?ticos dispon?veis na literatura. Os modelos de Mart?nez et al. (2003) e o Simple Single Plate (SSP) de Gaspar et al. (2003) representaram os dados experimentais com os menores erros quadr?ticos m?dios (MSE). O custo de manufatura de 17,85 US$/kg?leo foi estimado para produ??o do ?leo de linha?a utilizando o software TECANALYSIS e a metodologia de Rosa e Meireles (2005). Com o intuito de estabelecer compara??es com a EFS, foram realizados ensaios de extra??o por t?cnica convencional em aparato Soxhlet utilizando ?ter de petr?leo. Estes apresentaram rendimentos m?dios de 35,2 % para um tempo de extra??o de 5h. Todas as amostras de ?leo obtidas foram esterificadas e caracterizadas em termos de sua composi??o em ?cidos graxos (AGs) usando a cromatografia gasosa. Os principais ?cidos graxos detectados foram: palm?tico (C16:0), este?rico (C18:0), ol?ico (C18:1), linol?ico (C18:2n-6) e α-linol?nico (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 t?cnica Soxhlet com ?ter de petr?leo. Com rela??o ao teor do ?cido α-linol?nico (componente majorit?rio do ?leo de linha?a) nas amostras, a EFS se mostrou mais vantajosa que a extra??o Soxhlet, apresentando percentuais de 51,18 a 52,71%, enquanto que na extra??o Soxhlet, este foi de 47,84%. A atividade antioxidante do ?leo foi avaliada no sistema de co-oxida??o b-caroteno/?cido linol?ico. Os percentuais de inibi??o do processo oxidativo chegaram a 22,11% para o ?leo da EFS, sendo de apenas 6,09% para o ?leo comercial extra?do a frio, o que sugere que a t?cnica EFS preserva melhor os compostos fen?licos presentes na semente, compostos estes, provavelmente respons?veis pelo car?ter antioxidante do ?leo. Testes in vitro com a amostra de melhor resposta antioxidante foram realizados em homogenato de f?gado de ratos, de forma a investigar a inibi??o da peroxida??o lip?dica espont?nea ou autoxida??o do tecido biol?gico. O ?leo de linha?a se mostrou mais eficiente que o ?leo de peixe (usado como padr?o) na diminui??o da peroxida??o lip?dica do tecido hep?tico dos ratos Wistar, apresentando resultados equivalentes aos obtidos com o uso do BHT (antioxidante sint?tico). A capacidade inibit?ria pode ser atribu?da ? presen?a de compostos fen?licos com atividade antioxidante presentes no ?leo de linha?a. Os resultados obtidos indicam a necessidade de estudos mais aprofundados tendo em vista a import?ncia do ?leo de linha?a como uma das maiores fontes de ω3 dentre os ?leos vegetais

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