Extração de esqualeno do destilado da desodorização do óleo de soja modificado utilizando dióxido de carbono supercrítico

• Autor(a) principal: Wobeto, Carmen
• Data de Publicação: 2007
• Tipo de documento: Tese
• Idioma: por
• Título da fonte: LOCUS Repositório Institucional da UFV
• Texto Completo: http://locus.ufv.br/handle/123456789/503
• topic: Esqualeno; Extração supercrítica; Cromatografia gasosa; Desodorização de óleo; Squalene; Supercritical extraction; Gas chromatography; Oil deodorizer; CNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOS::CIENCIA DE ALIMENTOS

In this work the analytical extraction of squalene in soy oil deodorization distillate (SODD) by supercritical carbon dioxide (CO2-SC) was investigated. The matrix was previously submitted to crystallization at low temperatures and treatment with Na2CO3 (crystallization/Na2CO3). Four temperatures and two types of solvent were tested for crystallization of SODD. It was verified that the crystallization condition that yielded lower mass of non cristalizable (MNC) was storage in hexane and than in acetone, both at -40 oC. The physical-chemistry modifications of the SODD reduced in 41% the content of total phytosterols, also was removed 98,9% of free fatty acid (FFA) and the concentration of squalene increased in 84%. During the extraction with CO2-SC the following variables were kept constant: amount sample (15 mg), sample reconstitution solvent (n-hexane), temperature of the restrictor (55 oC), temperatures of the collector during the extraction (20 oC) and during the reconstitution of the sample (55 oC). For the optimization of the extraction with CO2-SC, the effect of three temperatures (40, 50 and 60 oC) and three pressures (110, 157 and 281 bar) was initially evaluated. It could be concluded that the highest pressure and the lowest temperature tested yielded the highest amount of extracted squalene (7.12 g/100 g), probably because of the highest density of the fluid (0.90 g/mL). Subsequently, two static extraction times (SET, 0 and 5 min), two CO2 flow rates (1 and 1.5 mL/min) and three dynamic extraction times (DET, 15, 20 and 25 min) were tested. The highest squalene amount (9.44 g/100 g) was obtained by using the highest flow rate and longest SET and DET. However the squalene levels (9.33 g/100 g) obtained with 5 min in SET, 15 min in DET and 1.0 mL/min CO2 flow rate did not differ significantly. Since more reduced times and flow rates are more economically viable, the optimized parameters for the extraction with CO2-SC were: 40 oC, 281 bar, 0.90 g/mL, 5 min (SET), 15 min (DET) and 1.0 mL/min CO2 flow rate. The methodology developed in this work provided a concentration of 2.8 times in the squalene content, therefore, a study on the cost/benefit ratio is recommended, as well as testing of pilot scale plant, in order to assess its industrial potential.