Obtenção de insumo farmacêutico a partir das folhas de Cissampelos sympodialis Eichl e seu efeito sobre mediadores inflamatórios relevantes para a asma

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior

Dispersões sólidas de sinvastatina: preparação, caracterização, no estado sólido utilizando técnicas emergentes e estudo de estabilidade

This thesis aimed to assess the increase in solubility of simvastatin (SINV) with solid dispersions using techniques such as kneading (MA), co-solvent evaporation (ES), melting carrier (FC) and spray dryer (SD). Soluplus (SOL), PEG 6000 (PEG), PVP K-30 (PVP) e sodium lauryl sulphate (LSS) were used as carriers. The solid dispersions containing PEG [PEG-2(SD)], Soluplus [SOL-2(MA)] and sodium lauryl sulphate [LSS-2(ES)] were presented with a greater increase in solubility (5.02, 5.60 and 5.43 times respectively); analyses by ANOVA between the three groups did not present significant difference (p<0.05). In the phase solubility study, the calculation of the Gibbs free energy (ΔG) revealed that the spontaneity of solubilisation of SINV occurred in the order SOL>PEG >PVP 75%>LSS, always 80%. The phase diagrams of PEG and LSS presented solubilization stoichiometry of type 1:1 (type AL). The diagrams with PVP and SOL tend to 1:2 stoichiometry (type AL + AP). The stability coefficients (Ks) of the phase diagrams revealed that the most stable reactions occurred with LSS and PVP. The solid dispersions were characterized by Fourier transform infrared (FTIR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), particle size distribution (PSD), near-infrared spectroscopy imaging (NIR-CI) and X-ray diffraction of the powder using the Topas software (PDRX-TOPAS). The solid dispersion PEG-2(SD) presented the greatest homogeneity and the lowest degree of crystallinity (18.2%). The accelerated stability study revealed that the solid dispersions are less stable than SINV, with PEG-2(SD) being the least stable, confirmed by FTIR and DSC. The analyses by PDRX-TOPAS revealed the amorphous character of the dispersions and the mechanism of increasing solubility

Heurísticas usando construção de vocabuilário aplicadas ao problema da atribuição de localidades a anéis em redes SONET/SDH

The SONET/SDH Ring Assignment Problem (PALAS) treats to group localities in form of some rings, being respected the traffic's limitations of the equipment. Each ring uses a DXC (Digital Cross Connect) to make the communication with the others, being the DXC the equipment most expensive of the net, minimizing the number total of rings, will minimize the total net cost, problem's objective . This topology in rings provides a bigger capacity of regeneration. The PALAS is a problem in Combinatorial Optimization of NP-hard Class. It can be solved through Heuristics and Metaheuristics. In this text, we use Taboo Search while we keep a set of elite solutions to be used in the formation of a part of the collection of vocabulary's parts that in turn will be used in the Vocabulary Building. The Vocabulary Building will be started case Taboo Search does not reach the best solution for the instance. Three approaches had been implemented: one that only uses vocabulary's parts deriving of Taboo Search, one that it only uses vocabulary's parts randomly generated and a last one that it uses half come of the elite and half randomly generated

Calibração cega de receptores cinco-portas baseada em separação cega de fontes

The exponential growth in the applications of radio frequency (RF) is accompanied by great challenges as more efficient use of spectrum as in the design of new architectures for multi-standard receivers or software defined radio (SDR) . The key challenge in designing architecture of the software defined radio is the implementation of a wide-band receiver, reconfigurable, low cost, low power consumption, higher level of integration and flexibility. As a new solution of SDR design, a direct demodulator architecture, based on fiveport technology, or multi-port demodulator, has been proposed. However, the use of the five-port as a direct-conversion receiver requires an I/Q calibration (or regeneration) procedure in order to generate the in-phase (I) and quadrature (Q) components of the transmitted baseband signal. In this work, we propose to evaluate the performance of a blind calibration technique without additional knowledge about training or pilot sequences of the transmitted signal based on independent component analysis for the regeneration of I/Q five-port downconversion, by exploiting the information on the statistical properties of the three output signals

Obtenção e caracterização de extrato microencapsulado de resíduo agroindustrial de acerola

Acerola (Malpighia emarginata D.C.) is a red fruit widely cultivated in Brazil, especially in the Northeastern region. Its increasing demand is attributed to its high ascorbic acid contents. Besides ascorbic acid, widely known by its health-benefit effects, acerola is rich in anthocyanins, which contribute for the antioxidant power of the fruit. Acerola processing produces a bright-red pomace, usually discarded. The further processing of this pomace, in order to explore its antioxidant compounds, could enhance acerola market value and rentability of its processing. Both ascorbic acid and anthocyanins are highly susceptible to degradation, that can be delayed by microencapsulation, which consists on packing particles (core) in an edible matrix (wall material). This work has been made with the purpose of producing a microencapsulated acerola pomace extract, which could be used by the food industry as a functional ingredient with antioxidant and coloring properties. Antioxidant compounds were recovered by pressing the pomace diluted in a solvent (a citric acid aqueous solution), by using a central composite design, with two variables: citric acid concentration in the solvent (0-2%), and solvent: pomace mass ratio (2:1-6:1). The acerola pomace extract was then microencapsulated by spray drying. A central composite design was adopted, with three variables: inlet temperature of the spray dryer (170o-200oC), wall material: acerola solids mass ratio (2:1-5:1), and degree of maltodextrin replacement by cashew tree gum as wall material (0-100%). The cashew tree gum was used because of its similarity to arabic gum, which is regarded as the wall material by excellence. The following conditions were considered as optimal for extraction of anthocyanins and ascorbic acid: solvent/pomace ratio, 5:1, and no citric acid in the solvent. 82.47% of the anthocyanins were recovered, as well as 83.22% of the ascorbic acid. Anthocyanin and ascorbic acid retentions were favored by lower inlet temperatures, higher wall material: acerola solids mass ratio and higher maltodextrin replacement by cashew tree gum, which was presented as a promising wall material. The more adequate microencapsulation conditions, based not only on retention of antioxidant compounds but also on physical properties of the final powder, were the following: inlet temperature, 185oC; wall material: acerola solids mass ratio, 5:1, and minimum degree of maltodextrin replacement by cashew tree gum, 50%

Extração do óleo e caracterização dos resíduos da borra de petróleo para fins de reuso

The petroleum industry, in consequence of an intense activity of exploration and production, is responsible by great part of the generation of residues, which are considered toxic and pollutants to the environment. Among these, the oil sludge is found produced during the production, transportation and refine phases. This work had the purpose to develop a process to recovery the oil present in oil sludge, in order to use the recovered oil as fuel or return it to the refining plant. From the preliminary tests, were identified the most important independent variables, like: temperature, contact time, solvents and acid volumes. Initially, a series of parameters to characterize the oil sludge was determined to characterize its. A special extractor was projected to work with oily waste. Two experimental designs were applied: fractional factorial and Doehlert. The tests were carried out in batch process to the conditions of the experimental designs applied. The efficiency obtained in the oil extraction process was 70%, in average. Oil sludge is composed of 36,2% of oil, 16,8% of ash, 40% of water and 7% of volatile constituents. However, the statistical analysis showed that the quadratic model was not well fitted to the process with a relative low determination coefficient (60,6%). This occurred due to the complexity of the oil sludge. To obtain a model able to represent the experiments, the mathematical model was used, the so called artificial neural networks (RNA), which was generated, initially, with 2, 4, 5, 6, 7 and 8 neurons in the hidden layer, 64 experimental results and 10000 presentations (interactions). Lesser dispersions were verified between the experimental and calculated values using 4 neurons, regarding the proportion of experimental points and estimated parameters. The analysis of the average deviations of the test divided by the respective training showed up that 2150 presentations resulted in the best value parameters. For the new model, the determination coefficient was 87,5%, which is quite satisfactory for the studied system

Extração do óleo essencial de Cymbopogom winterianus J. com CO2 pressurizado

The extraction with pressurized fluids has become an attractive process for the extraction of essential oils, mainly due the specific characteristics of the fluids near the critical region. This work presents results of the extraction process of the essential oil of Cymbopogon winterianus J. with CO2 under high pressures. The effect of the following variables was evaluated: solvent flow rate (from 0.37 to 1.5 g CO2/min), pressure (66.7 and 75 bar) and temperature (8, 10, 15, 20 and 25 ºC) on the extraction kinetics and the total yield of the process, as well as in the solubility and composition of the C. winterianus essential oil. The experimental apparatus consisted of an extractor of fixed bed and the dynamic method was adopted for the calculation of the oil solubility. Extractions were also accomplished by conventional techniques (steam and organic solvent extraction). The determination and identification of extract composition were done by gas chromatography coupled with a mass spectrometer (GC-MS). The extract composition varied in function of the studied operational conditions and also related to the used extraction method. The main components obtained in the CO2 extraction were elemol, geraniol, citronellol and citronellal. For the steam extraction were the citronellal, citronellol and geraniol and for the organic solvent extraction were the azulene and the hexadecane. The most yield values (2.76%) and oil solubility (2.49x10-2 g oil/ g CO2) were obtained through the CO2 extraction in the operational conditions of T = 10°C, P = 66.7 bar and solvent flow rate 0.85 g CO2/min

Tratamento de materiais contaminados com bifenilas policloradas (PCBS) via extração convencional e fluído supercrítico

The decontamination of the materials has been subject of some studies. One of the factors that it increases the pollution is the lack of responsibility in the discarding of toxic trash, as for example the presence of PCB (Polychlorinated Biphenyls) in the environment. In the Brazilian regulations, the material contaminated with PCB in concentrations higher than 50 ppm must be stored in special places or destroyed, usually by incineration in plasma furnace with dual steps. Due to high cost of the procedure, new methodologies of PCBs removal has been studied. The objective of this study was to develop an experimental methodology and analytical methodology for quantification of removal of PCBs through out the processes of extractions using supercritical fluid and Soxhlet method, also technical efficiency of the two processes of extraction, in the treatment of contaminated materials with PCBs. The materials studied were soils and wood, both were simulated contamination with concentration of 6.000, 33.000 and 60.000 mg of PCB/ kg of materials. Soxhlet extractions were performed using 100 ml of hexane, and temperature of 180 ºC. Extractions by fluid supercritical were performed at conditions of 200 bar, 70°C, and supercritical CO2 flow-rate of 3 g/min for 1-3 hours. The extracts obtained were quantified using Gas chromatography-mass spectrometry (GC/MS). The conventional extractions were made according to factorial experimental planning technique 22, with aim of study the influence of two variables of process extraction for the Soxhlet method: contaminant concentration and extraction time for obtain a maximum removal of PCB in the materials. The extractions for Soxhlet method were efficient for extraction of PCBs in soil and wood in both solvent studied (hexane and ethanol). In the experimental extraction in soils, the better efficient of removal of PCBs using ethanol as solvent was 81.3% than 95% for the extraction using hexane as solvent, for equal time of extraction. The results of the extraction with wood showed statistically it that there is not difference between the extractions in both solvent studied. The supercritical fluid extraction in the conditions studied showed better efficiency in the extraction of PCBs in the wood matrix than in soil, for two hours extractions the obtain percentual of 43.9 ± 0.5 % for the total of PCBs extracted in the soils against 95.1 ± 0,5% for the total of PCBs extracted in the wood. The results demonstrated that the extractions were satisfactory for both technical studied

Desenvolvimento de sistemas micro e nanoestruturados de quitosana/MDI para aplicações cosméticas

Currently, studies in the area of polymeric microcapsules and nanocapsules and controlled release are considerably advanced. This work aims the study and development of microcapsules and nanocapsules from Chitosan/MDI, using a new technique of interfacial polycondensation combined to spontaneous emulsification, for encapsulation of BZ-3. It was firstly elaborated an experimental design of 23 of the particle in white without the presence of BZ-3 and Miglyol, where the variables were the concentrations of MDI, chitosan and solvent. Starting from the data supplied by the experimental design was chosen the experiment with smaller particle diameter and only added like this BZ-3 and Miglyol. The suspension containing concentrations of 6.25 mg/mL, 12.5 mg/mL, 18.75 mg/mL, 25 mg/mL of BZ-3 were prepared, nevertheless, during the storage time, these formulations presented drug precipitates in the suspensions of 18.75 mg/mL and 25 mg/mL of BZ-3. This apparition of precipitate was attributed to the diffusion of BZ-3 for the aqueous phase without any encapsulation, suggesting so the use of the smaller concentrations of the BZ-3. The suspension containing 6.25mg/mL of BZ3 presented average size of 1.47μm, zeta potential of 61 mV, pH 5.64 and this sample showed an amount of BZ-3 and drug entrapment of 100 %. The suspension containing 12.5mg/mL of BZ-3 presented average size of 1.76μm, zeta potential of 47.4 mV, pH 5.71 and this sample showed an amount of BZ-3 and drug entrapment of 100 %. Then, showing such important characteristics, these two formulations were chosen for futher continuity to the study. These formulations were also characterized by the morphology, FTIR, stability for Turbiscan, DSC and a study of controlled release of the BZ-3 was elaborated in different receiving means

Purificação da glicerina bruta obtida a partir da transesterificação do óleo de algodão

The crude glycerine is a raw material that can be used in a wide variety of products. Even with all the impurities inherent in the process of being obtained, the crude glycerin is already in a marketable product. However, the market is much more favorable to the commercialization of purified glycerine. The glycerin is a byproduct gotten from the process of transesterification of waste oils and fats in the production of biodiesel. More recently, the deployment of the new Federal Law of Brazil, related to the implementation of energy resources, forces, from 2008, the increase of 2% biodiesel in diesel common with prospects for 5% (B5). Therefore, it is indispensable that new routes of purification as well as new markets are developed. The objective of this work was to purify, through ion exchange, the crude glycerin, obtained from the reaction of transesterification of cottonseed oil. The cottonseed oil was characterized as the fatty acid composition and physical-chemical properties. The process of ion exchange was conducted in batch. In this process were used strong cation, low anion resins and a mixed resin used to de-ionize water. The purified glycerin was characterized as the content of metals. Tests were performed with activated charcoal adsorption, and for this, it was made tests of time contact with coal as well as quantity of coal used. The time of activation, the amount of the activation solution, the contact time of the glycerol solution in resins, the amount and type of resin applied were evaluated. Considering the analysis made with activated charcoal, when the glycerin solution was treated using the resins individually it was observed that in the conditions for treatment with 10 g of resin, 5 hours of contact with each resin and 50 mL of glycerin solution, its conductivity decreased to a cationic resin, increased to the anionic resin and had a variable value with respect to resin mixed. In the treatment in series, there was a constant decrease in the conductivity of the solution of glycerin. Considering two types of treatment, in series and individually, the content of glycerol in glycerin pre-purified solution with the different resins varied from 12,46 to 29.51% (diluted solution). In analysis performed without the use of activated charcoal, the behavior of the conductivity of the solution of glycerin were similar to results for treatment with activated charcoal, both in series as individually. The solution of glycerin pre-purified had a glycerol content varying from 8.3 to 25.7% (diluted solution). In relation to pH, it had a behavior in accordance with the expected: acid for the glycerin solution treated with cationic resin, basic when the glycerin solution was treated with the anionic resin and neutral when treated with the mixed resin, independent of the kind of procedure used (with or without coal, resins individually or in series). In relation to the color of the glycerin pre-purified solution, the resin that showed the best result was the anionic (colorless), however this does not mean that the solution is more in pure glycerol. The chromatographic analysis of the solutions obtained after the passage through the resins indicated that the treatment was effective by the presence of only one component (glycerol), not considering the solvent of the analysis

Aplicação de microemulsões na solubilização de frações pesadas de petróleo

This work presents studies related to the use of microemulsions in the solubilization of heavy crude oil fractions responsible by the formation of deposits. The first stage of the work was addressed to the construction of phases diagrams, with the intention of determining the area within which the microemulsion is formed. The following systems were studied: UNITOL L 90 n-Butanol - Water - Kerosene (system 1); UNITOL L 90 - n-Butanol - Water - Xylene (system 2); UNITOL L 90 n-Butanol - Water - Kerosene/Xylene 10% (system 3); UNITOL L 90 - Sec-Butanol - Water - Xylene (system 4). In parallel experiments of physical adsorption were carried out by the static method, with the intention of simulating natural conditions of reservoirs. Crude oil of the Fazenda Belém field (Rio Grande do Norte), was used as solute, xylene as solvent and the Assu sandstone (Rio Grande do Norte, Brazil) and Botucatu sandstone (Paraná, Brazil) as rock reservoirs. The curves of adsorption presented the S format type, in agreement with the classification proposed by Giles, Smith and Huitson (1974). The solubilization process was accomplished in the batch method, by varying the time of agitation, the microemulsions and the solid/solution ratio. The experiments showed that the microemulsions presented high efficiency in the solubilization of the crude oil adsorbed on the sandstones. System 2 presented an efficiency of 99% for the Assu sandstone and 97% for the Botucatu sandstone

Controle feedback de nível baseado em sensor de imagem aplicado ao equipamento misturador-decantador à inversão de fases (MDIF®)

The treatment of wastewaters contaminated with oil is of great practical interest and it is fundamental in environmental issues. A relevant process, which has been studied on continuous treatment of contaminated water with oil, is the equipment denominated MDIF® (a mixer-settler based on phase inversion). An important variable during the operation of MDIF® is the water-solvent interface level in the separation section. The control of this level is essential both to avoid the dragging of the solvent during the water removal and improve the extraction efficiency of the oil by the solvent. The measurement of oil-water interface level (in line) is still a hard task. There are few sensors able to measure oil-water interface level in a reliable way. In the case of lab scale systems, there are no interface sensors with compatible dimensions. The objective of this work was to implement a level control system to the organic solvent/water interface level on the equipment MDIF®. The detection of the interface level is based on the acquisition and treatment of images obtained dynamically through a standard camera (webcam). The control strategy was developed to operate in feedback mode, where the level measure obtained by image detection is compared to the desired level and an action is taken on a control valve according to an implemented PID law. A control and data acquisition program was developed in Fortran to accomplish the following tasks: image acquisition; water-solvent interface identification; to perform decisions and send control signals; and to record data in files. Some experimental runs in open-loop were carried out using the MDIF® and random pulse disturbances were applied on the input variable (water outlet flow). The responses of interface level permitted the process identification by transfer models. From these models, the parameters for a PID controller were tuned by direct synthesis and tests in closed-loop were performed. Preliminary results for the feedback loop demonstrated that the sensor and the control strategy developed in this work were suitable for the control of organic solvent-water interface level

Extração e pirólise do óleo de girassol (Helianthus annus l.) visando a produção de biocombustíveis

Nowadays, the growing environmental worry leads research the focus the application of alternative materials from renewable resources on the industrial process. The most common vegetable oil extractant using around the world is the hexane, a petroleum derived, toxic and flammable. Based on this fact, the goal of this work was to test vegetable oil extractions from sunflower seeds cultivated on the Rio Grande do Norte State using two extraction process, the mechanical expelling and solvent extraction, this one using hexane and ethanol as a alternative solvent. The solvent extractions were carried out in the Soxhlet extractor in three different extraction times (4, 6, and 8 hours). The effect of solvent and extraction time was evaluated. The mechanical extraction was carried out in a expeller and the sunflower oil obtained was characterized by its physical-chemical properties and compared with sunflower refinery oil. Furthermore this work also explored the pyrolysis reaction carried out by thermogravimetry measurement as alternative route to obtain biofuel. For this purpose the oil samples were heated to ambient temperature until 900°C in heating rate of 5, 10, 20ºC min-1 with the objective evaluated the kinetics parameters such activation energy and isoconversion. The TG/DTG curves show the thermal profile decomposition of triglycerides. The curves also showed that antioxidant presents on the refinery oil not influence on the thermal stability of sunflower oil. The total yield of the extraction s process with hexane and ethanol solvent were compared, and the results indicated that the extraction with ethanol were more efficient. The pyrolysis reaction results indicated that the use of unpurified oil required less energy to obtain the bio-oil

Otimização do processo de recuperação do cromo de efluentes de curtumes por microemulsões no extrator Morris

The tanning industries are those which transform animal hide or skin into leather. Due to the complexity of the transformation process, greater quantities of chemicals are being used which results in the generation of effluents with residual solids. The chromium in the residual waters generated by tanning tend to be a serious problem to the environment, therefore the recovery of this metal could result in the reduction of manufacturing costs. This metal is usually found in a trivalent form which can be converted into a hexavalent compound under acidic conditions and in the presence of organic matter. The present study was carried out with the objective to recover chromium through an extraction/re-extraction process using micro emulsions. Micro emulsions are transparent and thermodynamically stable system composed of two immiscible liquids, one forming the continuous phase and the other dispersed into micro bubbles, established by an interfacial membrane formed by surface active and co-surface active molecules. The process of recovering the chromium was carried out in two stages. The first, an extraction process, where the chromium was extracted in the micro emulsion phase and the aqueous phase in excess was separated. In the second stage, a concentrated acid was added to the micro emulsion phase rich in chromium in order to obtain a Winsor II system, where the water that formed in the micro emulsion phase separates into a new micro emulsion phase with a higher concentration of chromium, due to the lowering of the hydrophiles as well as the ionisation of the system. During the experimental procedure, a study was initiated with a synthetic solution of chromium sulphate passing onto the effluent. A Morris extractor was used in the extraction process. Tests were carried out according to the plan and the results were analysed by statistical methods in order to optimise the main parameters that influence the process: the total rate of flow (Q), stirring speed (w) and solvent rate (r). The results, after optimization, demonstrated that the best percentuals in relation to the chromium extraction (99 %) were obtained in the following operational conditions: Q= 2,0 l/h, w= 425 rpm and r= 0,375. The re-extraction was carried out at room temperature (28 °C), 40 °C and 50°C using hydrochloric acid (8 and 10 M) and sulphuric acid (8 M) as re-extracting agents. The results obtained demonstrate that the process was efficient enough in relation to the chromium extraction, reaching to re-extraction percentage higher than 95 %.

Aplicação de ultrassons no deslocamento de petróleo em meio poroso

The objective of this study was to evaluate the displacement of petroleum/diesel solutions, at different concentrations, observing the effect of ultrasonic vibrations in fluids present in porous media to obtain an increase in oil production. The bubbles produced by ultrasound implode asymmetrically in the rock, generating liquid jets with high speed, displacing the oil present in porous media. The oil/diesel solutions were prepared with concentrations ranging from 20 g/L to 720 g/L in oil in relation to diesel and its viscosities were obtained in a Brookfield Rheometer RS2000, with temperature ranging from 25 to 55 °C. After, calculations were performed to obtain the activation energy data for oil/diesel solutions. For oil recovery experiments, cylindrical samples of porous rock (core samples), with resin around the perimeter and its two circular bases free to allow the passage of fluids, were first saturated with 2% KCl solution and after with oil solutions. The results of oil extraction were satisfactory for all studied solutions, being obtained up to 68% partial displacement with saline solution injection. The ultrasound system was used after saline injection, increasing oil displacement, with oil extractions ranging from 63% to 79%. During the experiments, it was observed the warming of core samples, helping to reduce the viscosity of more concentrated systems, and consequently enhancing the percentage of advanced recovery for all studied solutions