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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.
151

Characterization of Perphenazine and Scopolamine Aerosols Generated Using the Capillary Aerosol Generator

Li, Xihao 01 January 2006 (has links)
The characterization of perphenazine and scopolamine aerosols generated using the capillary aerosol generator (CAG) was reported. Variables including steady state power, the formulation vehicle, the drug concentration and the formulation flow rate were studied for their effects on the chemical stability and particle size of these drug aerosols.Stability-indicating HPLC and LC-MS assays were developed and validated for perphenazine and scopolamine, respectively. The chemical stability of each compound was investigated under a variety of stress conditions and the structure of degradation products was proposed.Perphenazine aerosols were generated from propylene glycol (PG) formulations with concentrations of 9, 48 and 90mM at formulation flow rates of 2.5 and 5.0µL/s at a series of steady state powers. At higher aerosolization powers, the low concentration formulation (9mM) degraded with dehalogenation being the major pathway. The size of perphenazine aerosols was between 0.4 to 0.6µm. Changing the solute concentration produced only small changes (~0.2µm) in perphenazine aerosol particle size. The formulation flow rate did not significantly affect the aerosol size.Scopolamine degraded significantly when aerosolized in PG formulations. It was possible to generate chemically stable scopolamine aerosols from ethanol formulations. Significant amounts of degradation products were formed only at or above 4.6W at 5.0µL/s. Hydrolysis and dehydration appeared to be the major degradation pathways at higher powers and low formulation flow rate. The MMAD of scopolamine aerosols was between 0.5 and 2.0µm from 8, 20 and 40mM formulations at 5.0 and 10.0µL/s. The size of scopolamine aerosols increased as a function of increasing the solute concentration. Increasing the formulation flow rate increased the linear velocity of the spray, thus the Reynolds number was increased and smaller particles were generated.
152

Atomization modeling of liquid jets using an Eulerian-Eulerian model and a surface density approach / Modélisation de l'atomisation des jets liquides avec un modèle Eulérien-Eulérien et une approche de densité de surface

Mandumpala devassy, Bejoy 25 January 2013 (has links)
Dans les moteurs à combustion interne, l'injection de carburant est une phase essentielle pour la préparation du mélange et la combustion. En effet, la structure du jet liquide joue un rôle essentiel pour la qualité du mélange du combustible avec le gaz. Le présent travail porte sur les phénomènes d'atomisation de jet liquides dans les conditions opératoires des moteurs diesel. Dans ces conditions, la morphologie du jet liquide comprend une phase liquide séparée (c'est à dire un noyau liquide) et une phase liquide dispersée (c'est à dire un spray). Ce manuscrit décrit les étapes de développement d'un nouveau modèle d'atomisation, pour un jet liquide à grande vitesse, basée sur une approche eulérienne diphasique. Le phénomène d'atomisation est modélisée par des équations définissant une densité de surface pour le noyau liquide en plus de celle des gouttelettes du spray. Ce nouveau modèle a été couplé avec un système d'équations diphasique et turbulent de type Baer-Nunziato. Le processus de rupture des ligaments et son éclatement subséquent en gouttelettes sont modélisés en utilisant des connaissances rassemblées à partir des expériences disponibles et des simulations numériques précises. Dans la région dense du jet de liquide, l'atomisation primaire est modélisée comme un processus de dispersion en raison de l'étirement turbulent de l'interface, à partir du côté du liquide en plus du côté du gaz. Différents cas tests académiques ont été effectués afin de vérifier la mise en œuvre numérique du modèle dans le code IFP-C3D. Enfin, le modèle est validé avec les résultats DNS récemment publiés dans des conditions typiques de moteurs Diesel à injection directe. / In internal combustion engines, the liquid fuel injection is an essential step for the air/fuel mixture preparation and the combustion process. Indeed, the structure of the liquid jet coming out from the injector plays a key role in the proper mixing of the fuel with the gas in the combustion chamber. The present work focuses on the liquid jet atomization phenomena under Diesel engine conditions. Under these conditions, liquid jet morphology includes a separate liquid phase (i.e. a liquid core) and a dispersed liquid phase (i.e. a spray). This manuscript describes the development stages of a new atomization model, for a high speed liquid jet, based on an eulerian two-phase approach. The atomization phenomenon is modeled by defining different surface density equations, for the liquid core and the spray droplets. This new model has been coupled with a turbulent two-phase system of equations of Baer-Nunziato type. The process of ligament breakup and its subsequent breakup into droplets are handled with respect to available experiments and high fidelity numerical simulations. In the dense region of the liquid jet, the atomization is modeled as a dispersion process due to the turbulent stretching of the interface, from the side of liquid in addition to the gas side. Different academic test cases have been performed in order to verify the numerical implementation of the model in the IFP-C3D software. Finally, the model is validated with the recently published DNS results under typical conditions of direct injection Diesel engines.
153

Desenvolvimento de micropartículas gastro-resistentes contendo azitromicina por spray-drying / Development of azithromycin gastric-resistance microparticles by spray-drying

Verones, Daniel Antonio Garbim 25 October 2010 (has links)
A azitromicina é um antibiótico da classe dos macrolídeos utilizado principalmente no tratamento de infecções de pele e do trato respiratório. Suas propriedades farmacocinéticas lhe conferem ampla distribuição e acumulação tecidual. Devido à sua baixa biodisponibilidade (37%) e instabilidade ao pH ácido, foram investigadas alternativas para o desenvolvimento de microparticulados com propriedade gastro-resistente para aplicação em diferentes formas farmacêuticas. As micropartículas de azitromicina foram obtidas pela técnica de secagem por pulverização (spray-drying) com o polímero pH-dependente Eudragit® L30-D55 e trietilcitrato como plastificante. O desenvolvimento experimental seguiu um planejamento fatorial tipo Box-Behnken de quatro variáveis em três níveis. As micropartículas foram caracterizadas pela densidade aparente, densidade compactada, fator de Hausner, índice de Carr, ângulo de repouso e cromatografia líquida. O processo de secagem foi avaliado pelo rendimento e recuperação da azitromicina. A partir das características físicas do microparticulado e o rendimento do processo foram escolhidas três micropartículas para avaliação mais detalhada, contendo 15, 30 e 45% de polímero de revestimento sobre a concentração de azitromicina dihidrato. Estas foram avaliadas por difração de raios-X, calorimetria, infra-vermelho, microscopia eletrônica de varredura e teste de dissolução. Os fatores que mais influenciaram o processo de secagem e obtenção das micropartículas foram a concentração de Eudragit® L30D-55 e a temperatura do ar de secagem, sendo que, quanto menor a concentração de polímero e maior a temperatura de secagem melhores foram os rendimentos do processo. A recuperação da azitromicina para todas as micropartículas foram superiores a 80%. As micropartículas apresentaram baixa densidade aparente, porém com propriedades de fluxo que variaram de bom a excelente na maioria das condições de preparação. As avaliações por calorimetria e difração de raios-X sugerem que a azitromicina está encapsulada. Isto pode ser confirmado por meio das imagens da microscopia eletrônica de varredura que revelaram estruturas esféricas e uniformes. As micropartículas com maiores concentrações de polímero apresentaram as melhores características com proteção gástrica, acima de 50%, e são candidatas promissoras para o desenvolvimento de formas farmacêuticas sólidas orais gastro-resistentes contendo azitromicina. / The azithromycin is an antibiotic of the macrolide class used in cutaneous and respiratory infections treatments. Its pharmacokinetics properties confer a large cell distribution and accumulation in tissues. Due to its small bioavailability (37%) and acid pH instability, alternatives to the development of gastric-resistance microparticles to be uses in different pharmaceuticals forms were investigated. Azithromycin microparticles were obtained through spray-drying technique with the pH-dependent polymer Eudragit® L30-D55 and triethyl citrate as plasticizer. The experimental development followed a factorial planning Box-Behnken with four factors in three levels. The microparticles were characterized by bulk density, tapped density, Hausner ratio, Carr index, repose angle and HPLC. The drying process was evaluated by azithromycin yield and recover. From the microparticles physics parameters and the process yield, three samples were chosen to be better evaluated. The samples contained 15, 30 and 45% of coat polymer over azithromycin dehydrate. They were evaluated by X-ray powder diffraction (XRPD), calorimetry, infrared, surface electronic microscopy (SEM) and dissolution assay. The factors that most affected the drying process and the microparticles development were Eudragit® L30D-55 concentration and drying air temperature, and lower was the polymer amount and higher was the drying air temperature, better was the process yield. The azithromycin recover for all microparticles were superior to 80%. The microparticles presented low bulk density, but good flow properties for the great part of the samples. The calorimetry and the XRPD evaluations suggest that azithromycin is encapsulated, what can be confirmed through SEM pictures, which showed uniform and spherical structures. The microparticles with higher polymers concentrations showed the best characteristics with gastric protection above 50% and they are promising candidates to the development of oral solid pharmaceutical forms containing gastro-resistant azithromycin.
154

Influência do processo de secagem por pulverização mecânica (spray dryer) no tamanho de partícula e densidade aparente do café solúvel. / The influence of the mechanical spray drying process on particle size and bulk density of instant coffee.

Esteves, Bruno Neves 27 November 2006 (has links)
O Brasil é um grande produtor e consumidor de café. A bebida é a segunda mais consumida no país. O café solúvel é uma alternativa para o consumo diário visto que dispensa todo aparato de preparo da bebida, sendo necessária apenas água quente. O tamanho de partícula seca está diretamente ligado à densidade aparente do produto. Foram realizados testes de secagem de extrato de café em spray-dryer com atomização por disco rotativo e fluxo co-corrente variando-se a temperatura do ar de entrada (140 - 170 °C) e rotação do disco atomizador (27000 - 33000 rpm). A análise de tamanho de partícula mostrou tendência de partículas maiores quanto menor a temperatura de secagem (26 - 36 µm). Notou-se a influência tanto da temperatura quanto da rotação do disco atomizador na análise da atividade de água. A densidade aparente não se mostrou significativamente alterada pelos parâmetros estudados nos experimentos. / Brazil is a big producer and consumer of coffee. The drink is the second most consumed in the country. Instant coffee is an alternative for daily consumption since it dispenses with all the apparatuses for preparing the drink, being necessary only hot water. The dry particle size is directly related to the bulk density of the product. Coffee extract drying tests were made in a co-current flow spray-dryer with atomization by disc with a varying inlet air temperature (140 - 170 °C) and disc velocity (27000 - 33000 rpm). The particle size analysis has shown the tendency for bigger particles to form at lower drying temperatures (26 - 36 µm). The influence of inlet air temperature and the atomizer disc spin velocity were noted in water activity analysis. The bulk density was not significantly modified by the parameters studied in the experiments.
155

Direct determination of lead in aerosol by slurry AAS.

January 1999 (has links)
Kin-Fai Ho. / Thesis (M.Phil.)--Chinese University of Hong Kong, 1999. / Includes bibliographical references (leaves [61-66]). / Abstracts in English and Chinese. / Contents / ACKNOWLEDGMENT / ABSTRACT / Chapter CHAPTER 1 --- INTRODUCTION / Chapter 1.1 --- Air Pollution in Hong Kong / Chapter 1.2 --- Brief introduction of Particulate Matter / Chapter 1.2.1 --- Total suspended particulates / Chapter 1.2.2 --- Respirable suspended particulates / Chapter 1.2.3 --- PM2.5 / Chapter 1.3 --- Lead in Air Particulate and its Harmful Effects on Human / Chapter 1.4 --- Air Sampling / Chapter 1.5 --- Sample Treatment / Chapter 1.5.1 --- Acid digestion method / Chapter 1.5.2 --- Slurry sampling method / Chapter 1.5.3 --- Comparison between acid digestion and slurry sampling method / Chapter 1.5.4 --- Chemical modification / Chapter CHAPTER 2 --- EXPERIMENTAL / Chapter 2.1 --- Apparatus / Chapter 2.2 --- Instrumental analysis / Chapter 2.2.1 --- Electrothermal atomic absorption spectrometry / Chapter 2.2.2 --- Background correction by the Zeeman effect / Chapter 2.3 --- Reagents / Chapter 2.4 --- Procedure / Chapter 2.4.1 --- Collection of air sample / Chapter 2.4.2 --- Treatment of sample collected on filter / Chapter 2.4.2.1 --- Digestion Procedure / Chapter 2.4.2.2 --- Procedure for Slurry Preparation / Chapter 2.4.3 --- Temperature program employed / Chapter 2.4.4 --- Sample introduction / Chapter 2.4.5 --- Determination of Lead in PM 2.5 by Acid Digestion Method / Chapter 2.4.6 --- Determination of Lead in PM 2.5 by Developed Method / Chapter 2.4.7 --- Study of particle size and suspension behavior of PM 2.5 in solvent / Chapter CHAPTER 3 --- RESULTS AND DISCUSSION / Chapter 3.1 --- Choice of filter for air sampling / Chapter 3.2 --- Choice of Solvents for Suspension of Air Particulates / Chapter 3.3 --- Ultrasonic agitation / Chapter 3.4 --- Effect of the sonication time / Chapter 3.5 --- Particle size and Effect of stabilization agents / Chapter 3.6 --- Effect of acid predigestion of the slurry sample / Chapter 3.7 --- Chemical Modification / Chapter 3.7.1 --- Use palladium as chemical modifier / Chapter 3.7.2 --- Amount of chemical modifier / Chapter 3.7.3 --- Effect of nitric acid / Chapter 3.8 --- Optimization of the graphite furnace temperature / Chapter 3.9 --- Effect of using platform / Chapter 3.10 --- Sample injection volume / Chapter 3.11 --- Recovery study of Lead in PM2.5 / Chapter 3.12 --- The limit of detection and precision of the developed method / Chapter CHAPTER 4 --- CONCLUSION / APPENDIX / REFERENCES
156

Création et éjection des gouttes de l'atomisation / Formation and ejection of atomization drops

Paré, Gounséti Nimonoka 07 September 2015 (has links)
Cette thèse traite des instabilités hydrodynamiques survenant dans les ligaments liquides en présence d’écoulement axial, afin de comprendre la formation des gouttes lors des processus d’atomisation. Il a été montré par des études précédentes que tout processus d’atomisation passe par l’étape de la formation des ligaments, qui se déstabilisent en gouttelettes. Le processus de fragmentation des ligaments est régi par deux instabilités : l’instabilité de Rayleigh-Plateau lorsque le ligament est infini, le phénomène du « end pinching », lorsque le ligament est semi-infini. Dans les deux cas le mécanisme responsable du pincement du ligament est la capillarité. Dans cette thèse, nous avons montré que, sous certaines conditions, le pincement du ligament peut être retardé ou évité : c’est le phénomène d’évitement de l’étranglement. Une exploration détaillée de la zone de constriction du ligament (là où le rayon est minimal), révèle des effets non linéaires liés à la viscosité du fluide : la couche visqueuse se développe, s’enroule puis décolle de l’interface sous forme de jet, en aval du cou avec formation d’anneau tourbillonnaire. L’écoulement dans cette zone du ligament est soumis à une accélération axiale correspondant à une baisse de la pression : c’est l’effet Venturi. Ce type d’écoulement a été étudié à travers l’instabilité du pont capillaire entre deux tubes, soumis à un écoulement axial. Tout au long de ces travaux, deux approches ont été utilisées : les simulations numériques et des observations expérimentales. L’essentiel des résultats présentés a fait l’objet de publication ou d’une soumission d’article. / This thesis deals with the hydrodynamic instabilities which occur in a liquid ligament in presence of axial flow. We investigate the formation of drops during the atomization process. Previous studies highlighted a common step to all types of atomization processes: the initial formation of the ligament which later evolves into droplets. The ligaments fragmentation process is governed by two possible instabilities: the “Rayleigh-Plateau” instability which is characteristic of an infinite ligament and the “end-pinching” phenomenon, which occurs in semi-infinite ligaments. In both cases, capillarity is the driving mechanism underlying the ligament segmentation. In this thesis we show that, under certain conditions, the liquid ligament can surprisingly escape from pinch-off through creation of a vortex ring (“escape phenomenon”). A detailed analysis of the constriction zone (neck of the ligament) during the “escape phenomenon” suggested that nonlinear effects associated to fluid viscosity might play an important role in the escape process. Both our experimental observations and numerical results confirmed the occurrence of the detachment of the viscous layer into a jet downstream of the neck through creation of a vortex ring, when fluid viscosity exceeds a threshold. Accordingly, the fluid in the constriction zone undergoes an axial acceleration associated to a decrease in the pressure: this is the so-called “Venturi effect”. This type of flow is characteristic of the instability which emerges at the capillary bridge between two tubes subjected to axial flow. Part of the results obtained were the subject of a publication or article submission.
157

CHARACTERIZATION OF ROTARY BELL ATOMIZERS THROUGH IMAGE ANALYSIS TECHNIQUES

Wilson, Jacob E. 01 January 2018 (has links)
Three methods were developed to better understand and characterize the near-field dynamic processes of rotary bell atomization. The methods were developed with the goal of possible integration into industry to identify equipment changes through changes in the primary atomization of the bell. The first technique utilized high-speed imaging to capture qualitative ligament breakup and, in combination with a developed image processing technique and PIV software, was able to gain statistical size and velocity information about both ligaments and droplets in the image data. A second technique, using an Nd:YAG laser with an optical filter, was used to capture size statistics at even higher rotational speeds than the first technique, and was utilized to find differences between serrated and unserrated bell ligament and droplet data. The final technique was incorporating proper orthogonal decomposition (POD) into image data of a side-profile view of a damaged and undamaged bell during operation. This was done to capture differences between the data sets to come up with a characterization for identifying if a bell is damaged or not for future industrial integration.
158

Optimization of Complex Thermal-Fluid Processes

January 2015 (has links)
abstract: First, in a large-scale structure, a 3-D CFD model was built to simulate flow and temperature distributions. The flow patterns and temperature distributions are characterized and validated through spot measurements. The detailed understanding of them then allows for optimization of the HVAC configuration because identification of the problematic flow patterns and temperature mis-distributions leads to some corrective measures. Second, an appropriate form of the viscous dissipation term in the integral form of the conservation equation was considered, and the effects of momentum terms on the computed drop size in pressure-atomized sprays were examined. The Sauter mean diameter (SMD) calculated in this manner agrees well with experimental data of the drop velocities and sizes. Using the suggested equation with the revised treatment of liquid momentum setup, injection parameters can be directly input to the system of equations. Thus, this approach is capable of incorporating the effects of injection parameters for further considerations of the drop and velocity distributions under a wide range of spray geometry and injection conditions. Lastly, groundwater level estimation was investigated using compressed sensing (CS). To satisfy a general property of CS, a random measurement matrix was used, the groundwater network was constructed, and finally the l-1 optimization was run. Through several validation tests, correct estimation of groundwater level by CS was shown. Using this setup, decreasing trends in groundwater level in the southwestern US was shown. The suggested method is effective in that the total measurements of registered wells can be reduced down by approximately 42 %, sparse data can be visualized and a possible approach for groundwater management during extreme weather changes, e.g. in California, was demonstrated. / Dissertation/Thesis / Doctoral Dissertation Mechanical Engineering 2015
159

Eugenol microencapsulado em carragena combinada com proteínas do leite, do farelo de arroz e albumina sérica bovina por atomização / Eugenol microencapsulated in carrageenan combined with milk protein, rice bran protein and bovine serum albumin by spray drying

Veiga, Ruth dos Santos da 10 December 2015 (has links)
O eugenol é um composto fenólico natural que apresenta atividade antioxidante e antimicrobiana e o seu uso como substituto de aditivos sintéticos em alimentos tem sido proposto. Contudo, pela sua instabilidade frente aos agentes externos (luz, oxigênio e calor), seu uso no processamento de alimentos é comprometido. Assim, a microencapsulação é uma alternativa viável para sua aplicação. Os objetivos deste trabalho foram avaliar o efeito da variação das condições operacionais do atomizador (temperatura do ar de entrada e vazão de alimentação) na obtenção de eugenol microencapsulado em carragena, e estudar a influência da combinação de carragena e proteína do farelo de arroz, albumina sérica bovina e proteína do soro de leite com baixo teor de lactose na microencapsulação de eugenol. Em uma primeira etapa, um Delineamento Composto Central Rotacional (DCCR) do tipo 22 com duas variáveis independentes (temperatura do ar de secagem e vazão de alimentação), três pontos centrais e quatro pontos axiais, foi desenvolvido para avaliar as condições operacionais de atomização. A quantificação do eugenol, recuperação (RE %) e a eficiência de encapsulação (EE %) foi avaliadada por espectrofometria UV-Vis e a morfologia por microscopia ótica. Na segunda etapa, a influência do uso de carragena em combinação com proteína do farelo de arroz, albumina sérica bovina e proteína do soro de leite com baixo teor de lactose foi avaliada por meio de um planejamento de mistura do tipo simplex-centroid. A caracterização das microcápsulas foi determinada pela RE % e EE % por Cromatografia Líquida de Alta Eficiência (CLAE), análise termogravimétrica acoplada à espectrofotometria de infravermelho e, morfologia por microscopia eletrônica de varredura. Para o DCCR, o valor máximo de RE% obtido foi de 12% e as condições operacionais estudadas não influenciaram significativamente (p > 0,05). Já a EE% variou de 18,0 a 84,8% e, o termo quadrático para vazão de alimentação apresentou influência significativa (p ≤ 0,05) na resposta avaliada. Para o planejamento simplex-centroid, o valor médio de RE % das microcápsulas variou de 37,9 a 104,5% e o de EE% de 0,0 a 79,4%, sendo que ambas as respostas foram influenciadas (p ≤ 0,05%) pelos agentes encapsulantes da formulação. A albumina sérica bovina apresentou boa propriedade de estabilização da suspensão (RE % = 86,5) e em combinação com proteína de farelo do arroz possibilitou maior EE % (79,4). As microcápsulas exibiram diâmetro médio entre 3,4 a 4,6 µm e a morfologia das microcápsulas produzidas com a combinação da albumina sérica bovina e a proteína do farelo de arroz apresentaram superfícies esféricas com ausência de fissuras ou deformações. As análises térmicas e de FTIR, confirmam a eficiência de encapsulação do processo, indicando uma possível interação entre os agentes encapsulantes e o eugenol. / Eugenol is a natural phenolic compound with antioxidant and antimicrobial activity and its use as substitute the synthetic additives in food has been suggested. However, due eugenol instability to extern agents (light, oxygen and hot), its use in food processing has been hampered. Therefore, microencapsulation is a viable alternative for your application. The aims of this work were evaluate the effect of variation of operating conditions of spray drying (inlet air temperature and feed flow rate) in obtainment eugenol microencapsulated in carrageenan, and study the influence of combination of carrageenan and protein from rice bran protein, bovine serum albumin and, whey protein with low lactose content in the eugenol microencapsulation. Composite Central Desing (CCD) of type 22 with two independent variables (inlet air temperature, and feed flow rate), three key points and four axial points, were developed to assess the operational conditions of spray dryer. Eugenol quantification, recovery (% ER) and encapsulation efficiency (EE%) of process were evaluated by UV-Vis spectrophotometry and morphology by optical microscopy. In the second stage of the study, the influence of the use of carrageenan in combination with rice bran protein, bovine serum albumin and whey protein with low lactose content was evaluated by simplex-centroid desing. Microcapsules were characterizated by Ultra Performance Liquid Chromatography (UPLC) (ER and EE%), thermogravimetric analysis coupled to the infrared spectrophotometry, and morphology by scanning electron microscopy (SEM). In the CCD, the maximum ER% value was 12% and the operating conditions studied did not influence significantly (p > 0.05). EE% varied from 18.0 to 84.8% and the quadratic term to feed flow rate presented significant influence (p ≤ 0.05) in the evaluated answer. In the simplex-centroid mixture desing the ER% average of microcapsules ranged from 37.9 to 104.5% and EE% 0.0 to 79.4%, being that both responses were influenced (p ≤ 0.05%) by encapsulating agents of formulation. Bovine serum albumin presented good stabilizing property of suspension (ER% = 86.5) and in combination with rice bran protein resulted greater EE% (79.4). Microcapsules exhibited a average diameter range from 3.4 to 4.6 µm and the microcapsules morphology produced combination with the bovine serum albumin and protein rice bran showed surface with absence no cracks or deformation. Thermal and FTIR analysis confirmed the encapsulation efficiency of the process, observed a possible interaction between the encapsulating agents and eugenol.
160

Eugenol microencapsulado em carragena combinada com proteínas do leite, do farelo de arroz e albumina sérica bovina por atomização / Eugenol microencapsulated in carrageenan combined with milk protein, rice bran protein and bovine serum albumin by spray drying

Veiga, Ruth dos Santos da 10 December 2015 (has links)
O eugenol é um composto fenólico natural que apresenta atividade antioxidante e antimicrobiana e o seu uso como substituto de aditivos sintéticos em alimentos tem sido proposto. Contudo, pela sua instabilidade frente aos agentes externos (luz, oxigênio e calor), seu uso no processamento de alimentos é comprometido. Assim, a microencapsulação é uma alternativa viável para sua aplicação. Os objetivos deste trabalho foram avaliar o efeito da variação das condições operacionais do atomizador (temperatura do ar de entrada e vazão de alimentação) na obtenção de eugenol microencapsulado em carragena, e estudar a influência da combinação de carragena e proteína do farelo de arroz, albumina sérica bovina e proteína do soro de leite com baixo teor de lactose na microencapsulação de eugenol. Em uma primeira etapa, um Delineamento Composto Central Rotacional (DCCR) do tipo 22 com duas variáveis independentes (temperatura do ar de secagem e vazão de alimentação), três pontos centrais e quatro pontos axiais, foi desenvolvido para avaliar as condições operacionais de atomização. A quantificação do eugenol, recuperação (RE %) e a eficiência de encapsulação (EE %) foi avaliadada por espectrofometria UV-Vis e a morfologia por microscopia ótica. Na segunda etapa, a influência do uso de carragena em combinação com proteína do farelo de arroz, albumina sérica bovina e proteína do soro de leite com baixo teor de lactose foi avaliada por meio de um planejamento de mistura do tipo simplex-centroid. A caracterização das microcápsulas foi determinada pela RE % e EE % por Cromatografia Líquida de Alta Eficiência (CLAE), análise termogravimétrica acoplada à espectrofotometria de infravermelho e, morfologia por microscopia eletrônica de varredura. Para o DCCR, o valor máximo de RE% obtido foi de 12% e as condições operacionais estudadas não influenciaram significativamente (p > 0,05). Já a EE% variou de 18,0 a 84,8% e, o termo quadrático para vazão de alimentação apresentou influência significativa (p ≤ 0,05) na resposta avaliada. Para o planejamento simplex-centroid, o valor médio de RE % das microcápsulas variou de 37,9 a 104,5% e o de EE% de 0,0 a 79,4%, sendo que ambas as respostas foram influenciadas (p ≤ 0,05%) pelos agentes encapsulantes da formulação. A albumina sérica bovina apresentou boa propriedade de estabilização da suspensão (RE % = 86,5) e em combinação com proteína de farelo do arroz possibilitou maior EE % (79,4). As microcápsulas exibiram diâmetro médio entre 3,4 a 4,6 µm e a morfologia das microcápsulas produzidas com a combinação da albumina sérica bovina e a proteína do farelo de arroz apresentaram superfícies esféricas com ausência de fissuras ou deformações. As análises térmicas e de FTIR, confirmam a eficiência de encapsulação do processo, indicando uma possível interação entre os agentes encapsulantes e o eugenol. / Eugenol is a natural phenolic compound with antioxidant and antimicrobial activity and its use as substitute the synthetic additives in food has been suggested. However, due eugenol instability to extern agents (light, oxygen and hot), its use in food processing has been hampered. Therefore, microencapsulation is a viable alternative for your application. The aims of this work were evaluate the effect of variation of operating conditions of spray drying (inlet air temperature and feed flow rate) in obtainment eugenol microencapsulated in carrageenan, and study the influence of combination of carrageenan and protein from rice bran protein, bovine serum albumin and, whey protein with low lactose content in the eugenol microencapsulation. Composite Central Desing (CCD) of type 22 with two independent variables (inlet air temperature, and feed flow rate), three key points and four axial points, were developed to assess the operational conditions of spray dryer. Eugenol quantification, recovery (% ER) and encapsulation efficiency (EE%) of process were evaluated by UV-Vis spectrophotometry and morphology by optical microscopy. In the second stage of the study, the influence of the use of carrageenan in combination with rice bran protein, bovine serum albumin and whey protein with low lactose content was evaluated by simplex-centroid desing. Microcapsules were characterizated by Ultra Performance Liquid Chromatography (UPLC) (ER and EE%), thermogravimetric analysis coupled to the infrared spectrophotometry, and morphology by scanning electron microscopy (SEM). In the CCD, the maximum ER% value was 12% and the operating conditions studied did not influence significantly (p > 0.05). EE% varied from 18.0 to 84.8% and the quadratic term to feed flow rate presented significant influence (p ≤ 0.05) in the evaluated answer. In the simplex-centroid mixture desing the ER% average of microcapsules ranged from 37.9 to 104.5% and EE% 0.0 to 79.4%, being that both responses were influenced (p ≤ 0.05%) by encapsulating agents of formulation. Bovine serum albumin presented good stabilizing property of suspension (ER% = 86.5) and in combination with rice bran protein resulted greater EE% (79.4). Microcapsules exhibited a average diameter range from 3.4 to 4.6 µm and the microcapsules morphology produced combination with the bovine serum albumin and protein rice bran showed surface with absence no cracks or deformation. Thermal and FTIR analysis confirmed the encapsulation efficiency of the process, observed a possible interaction between the encapsulating agents and eugenol.

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