7 research outputs found

    Encapsulamento de B-caroteno em PHBV com dióxido de carbono e avaliação da liberação in vitro

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    Tese (doutorado) - Universidade Federal de Santa Catarina, Centro Tecnológico, Programa de Pós-Graduação em Engenharia de Alimentos, Florianópolis, 2011O objetivo geral desta tese foi estudar o processo de encapsulamento de ß-caroteno em PHBV (poli 3-hidroxibutirato-co-hidroxivalerato) utilizando dióxido de carbono pressurizado como anti-solvente avaliando, posteriormente, o comportamento de liberação in vitro das partículas. Para o alcance de tal objetivo, primeiramente, foi realizado um estudo do efeito das variáveis de processo nas características das partículas de ß-caroteno e PHBV, puras e co-precipitadas. Na precipitação do PHBV puro, o efeito da pressão foi verificado, avaliando-o na faixa de 80 a 200 bar e constatou-se que o aumento da pressão de precipitação tende a formar menores partículas. A morfologia não foi influenciada pela ação desta variável, apenas obteve-se comportamento diferente do PHBV não processado, o qual inicialmente tinha formação fibrosa passando após a precipitação para estrutura do tipo esfera. Para o ß-caroteno puro foi investigado o efeito da sua concentração na solução e também da pressão de precipitação, os quais foram de 4 e 8 mg.ml-1 e 80 a 200 bar, respectivamente. Verificou-se que mantendo a concentração da solução fixa, ocorre um aumento do tamanho médio das partículas de ß-caroteno com o aumento da pressão e que no intervalo de pressão de 80 a 160 bar as partículas apresentaram valores crescentes e na faixa de 160 a 200 bar o valor médio do tamanho das partículas decresceu. Na etapa de encapsulamento foram estudadas concentrações de ß-caroteno na solução que variaram de 2 a 30 mg.ml-1 sempre mantendo a concentração de PHBV fixa e igual a 30 mg.ml-1. Os percentuais e eficiência de encapsulamento foram determinados submetendo as amostras do material co-precipitado à agitação manual por 20 segundos e agitação magnética por 300 segundos, a partir do qual obteve-se eficiência máxima de encapsulamento de 55,53 % e 45,06 % respectivamente, na concentração de 30 mg.ml-1 de ß-caroteno. Observou-se na faixa de concentração de 8 a 16 mg.ml-1 de ß-caroteno um comportamento exponencial da eficiência de encapsulamento em função da sua concentração na solução. Os experimentos em que se obtiveram os maiores percentuais e eficiência de encapsulamento foram selecionados para o estudo dos ensaios de liberação em meios puros (acetato de etila, n-hexano, etanol anidro e solução tampão fosfato # pH 7,4) à 40 °C ± 0,5 °C e 80 rpm. Constatou-se que em acetato de etila e n-hexano os comportamentos de liberação são semelhantes e caracterizados por um burst inicial (em aproximadamente 10 minutos), na qual grande parte do princípio ativo foi liberada. Em média, foram obtidos percentuais de liberação que variaram de 26,97 % a 71,15 %, e de 42,09 % a 55,96 %, para os meios puros contendo acetato de etila e n-hexano, respectivamente. Em etanol anidro o comportamento de liberação apresentou-se diferente, pois não foi verificado o burst inicial e a liberação ocorreu de forma gradual e lenta, atingindo percentuais e tempos de liberação de até 88,22 % e 16 dias, respectivamente. Os resultados encontrados para os ensaios de liberação em solução tampão fosfato (pH 7,4) indicaram que mesmo após 60 dias, o princípio ativo continuou a ser liberado. Enfim, para todos os ensaios de liberação constatou-se que a concentração do princípio ativo liberada foi proporcional à massa inicial de ß-caroteno e que através dos meios usados pode-se optar por liberações rápidas ou prolongadas.The main objective of this work was to determine the in vitro release profiles of â-carotene microparticles encapsulated in PHBV through the use of supercritical fluid technology, using pressurized carbon dioxide as anti-solvent. For this purpose, at first, a study of the effect of process variables on the characteristics of the particles of â-carotene and PHBV, pure and co-precipitated was carried out. In the precipitation of pure PHBV, the effect of pressure was evaluated in the range from 80 to 200 bar, with a resulting negative effect on the particles average size. The morphology was not affected by this variable, leading to only a different behavior compared to raw PHBV, which initially had fibrous structure and after processing presented spherical type. For pure â-carotene, it was investigated the effect of concentration in the solution and also the precipitation pressure (4 and 8 mg.ml-1 and 80 to 200 bar, respectively). The results indicated that keeping the concentration of the solution fixed, there was an increase in the average size of â-carotene particles with increasing pressure and that the system pressure, in the range from 80 to 160 bar, promoted an increase in particle size and in the range of 160 to 200 bar, the mean particle size decreases. In the co-precipitation, it was studied the effect of â-carotene concentrations in solution (ranging from 20 to 30 mg.ml-1), keeping the concentration of PHBV fixed to 30 mg.ml-1. The percentage and encapsulation efficiency were analyzed submitting samples of the material co-precipitated to manual agitation (20 seconds) and magnetic stirring (300 seconds), with the maximum efficiency of encapsulation of 55.53% and 45.06%, respectively, for the â-carotene concentration of 30 mg.ml-1. An exponential behavior of the encapsulation efficiency depending on the â-carotene concentration (from 8 to 16 mg.ml-1) was also verified. The experiments that presented the highest percentage and encapsulation efficiency were selected for the study of the in vitro release, using pure solvent media (ethyl acetate, n-hexane, anhydrous ethanol and phosphate buffer - pH 7.4) at 313.15K and 80 rpm. It was observed that in ethyl acetate and n-hexane the release behaviors are similar and characterized by an initial burst (in about 10 minutes). In these solvents, the percentage of release ranged from 26.97 % to 71.15 %, and 42.09 % to 55.96 %, respectively. For anhydrous ethanol the release behavior was different because it was verified a gradual and slow release with percentage and release times of up to 88.22% and 16 days, respectively. The release results in phosphate buffer (pH 7.4) showed that even after 60 days the active principle continued to be released. For all tests, it was verified that the concentration of â-carotene released is proportional to the initial mass of this active principle and that the specific medium may be used to provide rapid or prolonged releases

    <b>Extraction of total polyphenols from hibiscus (<i>Hibiscus sabdariffa</i> L.) and waxweed / ‘sete-sangrias’ (<i>Cuphea carthagenensis</i>) and evaluation of their antioxidant potential

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    Current research investigates the extraction process of total polyphenols from hibiscus (Hibiscus sabdariffa L.) and waxweed (Brazilian name: ‘sete-sangrias’) (Cuphea carthagenensis) and evaluates the antioxidant potential of their extracts. The extraction stage comprised investigation on the following parameters: i) solvents (acetone and ethanol) pure and fractioned with water; ii) variables (temperature, stirring, solvent ratio, time and pH). Total polyphenols were quantified by Folin-Ciocalteau reagent and antioxidant activity was determined by ABTS•+ (2,2′-Azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) and DPPH (2,2-diphenyl-1-picrylhydrazyl) radical scavenging assay. Results showed that, depending on experimental conditions, total phenolic contents for hibiscus and waxweed ranged between 460.86 mg GAE 100 g-1 and 5012.54 mg GAE 100 g-1 and between 462.86 mg GAE 100 g-1 and 4215.99 mg GAE 100 g-1, respectively. Waxweed had a higher antioxidant activity when compared to that of hibiscus by both ABTS•+ and DPPH. Data showed that hibiscus and waxweed have a significant amount of polyphenols which may be extracted in mild processing conditions and then employed as natural antioxidant sources in industrial processes

    Micronization processes by supercritical fluid technologies: a short review on process design (2008-2012) - doi: 10.4025/actascitechnol.v35i4.18819

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    Several micronization processes based on supercritical fluids have been developed. These processes can be classified according to the role of the supercritical fluid in the process: solvent, solute or co-solvent, and anti-solvent. Application of supercritical fluids as alternative to traditional micronization methods and the growing demand of the industrial sector for new technologies motivated this review. In this context, the objective of this work was to present the operating principles of the micronization process by means of supercritical fluids and the effects of the main process variables on particles characteristics. The review continues with an update of current experimental data presented in the literature in the period from 2008 to 2012.  

    Modeling of the controlled release of betacarotene into anhydrous ethanol from microcapsules

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    In this paper several models of the mass transfer process are described with the aim of simulating the release of active principles from matrix-type polymeric microcapsules. The following mathematical models, which are available in the literature, are applied in this study: Fick's second law (CDMASSA), the linear drive force (LDF), an analytical model and other semi-empirical models. The release of the active principle (betacarotene) contained in microcapsules (PHBV) into a solvent (ethanol) was investigated. It was observed that the model obtained with Fick's second law provided a better fit with the literature data compared with the LDF model, the analytical model and the semi-empirical models. It can be concluded from this finding that the most complete model, based on the phenomenology of the problem, provided the best result
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