Submitted by Sandra Pereira (srpereira@ufrrj.br) on 2017-04-27T13:51:34Z No. of bitstreams: 1 2012 - Andr? Luis R. de Souza.pdf: 1971622 bytes, checksum: 5237bc23d365c59e774d9f8776efabf1 (MD5) / Made available in DSpace on 2017-04-27T13:51:34Z (GMT). No. of bitstreams: 1 2012 - Andr? Luis R. de Souza.pdf: 1971622 bytes, checksum: 5237bc23d365c59e774d9f8776efabf1 (MD5) Previous issue date: 2012-03-06 / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico - CNPq / Camu-camu is a native fruit from the Amazonian region, cultivated in the margins of rivers, lakes and Amazonian creeks called igarap?s. It is known as one of the fruit with the highest content of vitamin C. Reverse osmosis is a membrane concentration process in which the applied pressure is higher than the juice osmotic pressure. Such process favors the solvent permeation from the region with the highest concentration to the one with the lowest. Osmotic evaporation is another membrane concentration process in which a porous hydrophobic membrane separates the solution that is going to be concentrated from a concentrate brine solution. Microencapsulation is the process in which an active agent is entrapped by means of a polymer cover. Such process promotes the release of these active agents under specific conditions. The aim of this work is to evaluate the use of membrane separation processes and microencapsulation for the processing of camu-camu fruits. The camu-camu pulp, which has been obtained through the depulping of camu-camu fruits, was first centrifuged, in order to decrease its suspended solids content, and clarified by microfiltration with polysulfone membranes. Six clarification processes have carried out at 2.5 bar transmembrane pressure and 45?C. The clarified juice was concentrated by reverse osmosis at 60 bar and 20 ?C. The avarage permeate flux has been of 11.3 L/hm2. The preconcentrated juice had 28.8?Brix and the concentration degree of the process was 3.8. The pre-concentrated juice has been concentrated by osmotic evaporation in a laboratorial system with polytetrafluoroethylene membrane. The process presented an average pemeate flux of 2.4 Kg/hm2. The soluble solids content of the concentrated juice was of 56.6 ?Brix, presenting a concentration degree of 1.98. The retentate fraction of the microfiltration process was microencapsulated in a spray dryer. Three encapsulation agents were evaluated: starch, maltodextrin and the mixture of both. The values presented for the physicochemical caracterization of the pre-concentrated and concentrated camu-camu juices indicate that there has been an increase both in the physical characteristics of the juice, such as soluble solids, total solids and acidity, and in the concentration of camu-camu bioactive compounds. The dehydrated camu-camu juice presented a high concentration of bioactive substances. Nevertheless, there has been no stability of such compounds during storage. Through the results obtained in the present work, it is possible to observe that the integration of membrane processes proved efficient in the concentration of camu-camu juice, with a final product of high nutritional value / O camu-camu ? um fruto nativo da regi?o amaz?nica, cultivado as margens de rios, lagos e igarap?s. ? reconhecido como um dos frutos com um dos maiores teores de vitamina C. Osmose inversa ? o processo de concentra??o por membranas onde a press?o aplicada ? maior que a press?o osm?tica do suco, favorecendo a permea??o do solvente da regi?o de maior concentra??o para regi?o de menor concentra??o. Evapora??o osm?tica ? um outro processo de concentra??o, onde uma membrana hidrof?bica porosa separa a solu??o que ser? concentrada e uma salmoura concentrada. A microencapsula??o ? o processo onde um agente ativo ? protegido por meio de uma cobertura de pol?meros, ocorrendo a libera??o desses agentes ativos em condi??es espec?ficas. O objetivo desta disserta??o foi avaliar o uso dos processos de separa??o com membranas e microencapsulamento para o processamento de suco de camu-camu. Os frutos de camu-camu foram despolpados, sendo o suco submetido a centrifuga??o, com o objetivo de reduzir os s?lidos em suspens?o, e posteriormente clarificado por microfiltra??o em um sistema de membranas de polissulfona. Foram realizados seis processos de clarifica??o a 2,5 bar e 45?C. O suco clarificado foi pr?-concentrado por osmose inversa a 60 bar e 20 ?C. O fluxo permeado m?dio foi de 11,3 L/hm2. O suco pr?-concentrado apresentou teor de s?lidos sol?veis de 28,8?Brix e grau de concentra??o de 3,8. O suco pr?-concentrado foi processado por evapora??o osm?tica em um sistema laboratorial constitu?do por membranas de politetrafluoretileno. O processo apresentou fluxo m?dio permeado de 2,4 kg/hm2. O teor de s?lidos sol?veis do suco concentrado foi de 56,6 ?Brix, apresentando um grau de concentra??o de 1,98. O processo de microencapsula??o da fra??o retida do suco de camucamu foi realizado em um spray dryer Buchi Modelo B-190. Foram realizados tr?s ensaios com tr?s formula??es diferentes: mistura entre amido e maltodextrina, somente amido e somente maltodextrina. Os valores apresentados para a caracteriza??o f?sico-qu?mica do suco de camu-camu pr?-concentrado e concentrado indicam que houve um aumento nos s?lidos sol?veis e totais e da acidez, bem como no teor das subst?ncias bioativas do camucamu. O suco de camu-camu desidratado apresentou alto teor de subst?ncias bioativas, onde a estabilidade desses compostos durante o per?odo de armazenamento n?o foi alcan?ada. Observa-se que a integra??o dos processos com membranas se mostrou eficaz na concentra??o do suco de camu-camu, obtendo um produto com alta qualidade nutricional.

Hibiscus sabdariffa L. est une plante vivace herbacée localisée dans les zones tropicales et subtropicales des deux hémisphères. Au Sénégal, où elle a été introduite au 19ème siècle, H. sabdariffa, encore appelé bissap ou roselle, est cultivé sur l'ensemble du territoire et exploité principalement pour ses calices. Une boisson désaltérante est traditionnellement élaborée à partir des calices séchés par extraction à l'eau. La caractérisation physico-chimique et biochimique des calices nous a tout d'abord permis de mieux évaluer le potentiel de ce produit. Ainsi, les calices contiennent entre 767 et 1480 mg.100g -1 d'anthocyanes et entre 1347 et 3736 mg.100g-1 de polyphénols totaux. Ils présentent un pouvoir antioxydant voisin de 260 µmolTrolox.g-1. L'acide malique y est l'acide organique majoritaire avec une teneur pouvant atteindre 2,3 g.100g-1. De part ces caractéristiques, l'extrait aqueux de calices d'H. sabdariffa constitue une excellente source d'anthocyanes. Le travail s'est ensuite focalisé sur le procédé d'obtention de cet extrait. L'étude de l'extraction solide-liquide a été réalisée à partir de calices séchés et d'eau à des températures comprises entre 25 et 90 °C. Un rendement d'extraction en anthocyanes maximum de 88 % a été obtenu à 25 °C avec un ratio calice/eau de 1/25. La réduction de la taille des particules et l'augmentation de la température diminuent le temps d'extraction mais n'affectent pas le rendement d'extraction. Un modèle d'extraction solide-liquide incluant les cinétiques de dégradation thermique des anthocyanes a été proposé puis validé. La microfiltration tangentielle sur membrane céramique de diamètre moyen de pores 0,2 µm a permis de produire un extrait stérilisé à froid, stable pendant 90 j à 20 °C. Nous avons montré à ce niveau que la pression transmembranaire optimisée à un facteur de réduct ion volumique (FRV) égal à 1 n'est plus optimale lorsque le FRV augmente. Pour concentrer les anthocyanes présents dans l'extrait, l'ultrafiltration sur une membrane de seuil de coupure de 5 kDa peut être utilisée malgré une rétention incomplète (95-97 %). Par contre, la nanofiltration offre une rétention totale des anthocyanes. Le procédé, mis en uvre dans des conditions semi-industrielles, a permis d'augmenter la teneur en extrait sec soluble (ESS) de 40 à 250 g.kg-1 à 35 °C, à une pression transmembranaire comprise entre 20 et 30 bar avec un flux moyen de 15 kg.h-1.m-2. L'évaporation osmotique, testée sur un pilote équipé d'une membrane en polypropylène de 10 m2, a permis de concentrer l'extrait anthocyanique jusqu'à 620 g d'ESS.kg-1. Cet extrait concentré conserve toutes les qualités physico-chimiques, biochimiques, nutritionnelles et aromatiques de l'extrait initial. Le flux évaporatoire est directement corrélé à la teneur en extrait sec solub le du produit à concentrer. Enfin, divers couplages d'opérations unitaires ont été comparés pour obtenir un extrait concentré à partir de calices d'H. sabdariffa. Le procédé qui associe une extraction à froid, une pré-concentration par nanofiltration et une concentration par évaporation osmotique est la meilleure voie tant en terme de coûts d'investissement et de fonctionnement que de qualité de l'extrait. / Hibiscus sabdariffa L. is a herbaceous plant, cultivated largely in tropical and subtropical areas of both hemispheres. In Senegal, where it was introduced in the 19th century, H. sabdariffa L. also called bissap or roselle is grown throughout the territory and operated primarily for its calyx. A refreshing drink is traditionally made from dried calyx by water extraction. The physical-chemical and biochemical characterization of the calyx allowed us to assess better the potential of this product. Thus, the calyx contained between 767 and 1480 mg.100g-1 of anthocyanins and between 1347 and 3736 mg.100g-1 of total polyphenols. They have an antioxidant capacity closed to 260 μmolTrolox.g-1. Malic acid is the major organic acid with content up to 2.3 g.100g-1. Because of these characteristics, the aqueous extract of H. sabdariffa calyx is an excellent source of anthocyanins. The work was then focused on the process for obtaining this extract. The study of solid-liquid extraction was performed from dried calyx with water at temperature range from 25 and 90 ° C. A maximum extraction yield of anthocyanin of 88 % was obtained at 25 ° C with a solid-to-solvent ratio of 1/25. Reducing the particle size and increasing the temperature decreased the extraction time but do not affect the extraction efficiency. A model of solid-liquid extraction which included the thermal anthocyanins degradation kinetics has been proposed and validated. Crossflow microfiltration with tubular ceramic 0.2 pore size membrane has produced a cold sterilized extract, stable during 90 days at 20 °C. We have shown here that the transmembrane pressure optimized at a volume reduction ratio (VRR) equal to 1 is no longer optimum when the VRR is increasing. To concentrate the anthocyanins present in the extract, the ultrafiltration membrane with a cutoff of 5 kDa can be used despite incomplete retention (95-97%). By cons, nanofiltration offers a tot al retention of anthocyanins. The method, implemented in semi-industrial conditions, has increased the content of total soluble solids (TSS) from 40 to 250 g.kg-1 at 35 °C at a transmembrane pressure between 20 and 30 bar with an average flow of 15 kg.h-1.m-2. The osmotic evaporation, tested on a pilot equipped with a polypropylene membrane of 10 m2, has concentrated anthocyanin extract up to 620 g TSS. kg-1. This concentrated extract retains all the physical-chemical, biochemical, nutritional and aromatic quality of the original extract. The evaporation flux is directly correlated with the total soluble solids content of the product to concentrate. Finally, various couplings of unit operations were compared to obtain a concentrated extract from H. sabdariffa calyx. The process which combines a cold extraction, a pre-concentration by nanofiltration and concentration by osmotic evaporation is the best way both in terms of investment costs and operating and quality of the ext ract.