Desenvolvimento de metodologias analíticas alternativas por cromatografia gasosa para análise de biodiesel

Since the beginning of the National Program for Production and Use of Biodiesel in Brazil, in 2004, different raw materials were evaluated for biodiesel production, trying to combine the agricultural diversity of the country to the desire to reduce production coasts. To determine the chemical composition of biodiesel produced from common vegetables oils, international methods have been used widely in Brazil. However, for analyzing biodiesel samples produced from some alternative raw materials analytical problems have been detected. That was the case of biodiesel from castor oil. Due the need to overcome these problems, new methodologies were developed using different chromatographic columns, standards and quantitative methods. The priority was simplifying the equipment configuration, realizing faster analyses, reducing the costs and facilitating the routine of biodiesel research and production laboratories. For quantifying free glycerin, the ethylene glycol was used in instead of 1,2,4-butanetriol, without loss of quality results. The ethylene glycol is a cheaper and easier standard. For methanol analyses the headspace was not used and the cost of the equipment used was lower. A detailed determination of the esters helped the deeper knowledge of the biodiesel composition. The report of the experiments and conclusions of the research that resulted in the development of alternative methods for quality control of the composition of the biodiesel produced in Brazil, a country with considerable variability of species in agriculture, are the goals of this thesis and are reported in the following pages

Pesquisa odontológica no Brasil: características da produção científica no início do século XXI

Dentistry, as a science and field of knowledge, has presented a substantial development in the last decades in the areas of research and education. The aim of this study was to evaluate the Brazilian scientific production in Dentistry, as from their methodological outlining, which characterizes the XXI Century. Five thousand two hundred and three study abstracts were evaluated, comprising works presented in the meetings of the Brazilian Society of Dentistry Research (SBPqO), during the period of 2001 to 2006. The main results identify that, as for the methodology used in the researches, there was a predominance of the studies of an individuate, interventionist and longitudinal nature; of the researches in the areas of Dentistry, Periodontology, Endodontics, Pedodontics and Collective Oral Health and experimental studies about clinical researches or with collective subjects. The inter and multidisciplinarity are pointed out in the outlining of this study, as the triad Education-Health-Research is discussed, so that they transcend in their fields of action, in the direction of the transdisciplinarity. It is concluded that, in the studied period, there was a reasonable and balanced production in Brazilian dental field

Avaliação da qualidade da assistência a pessoas com úlceras venosas atendidas na estratégia saúde da família

A úlcera venosa constitui importante problema de saúde pública, gera repercussão social, econômica e mudanças nos hábitos de vida, dor, sofrimento, acarretando diminuição da qualidade de vida. O estudo objetivou avaliar a assistência prestada às pessoas com úlceras venosas atendidas pela Estratégia Saúde da Família. É um estudo analítico, transversal e quantitativo, realizado com 59 pessoas com úlceras venosas, atendidas em 36 unidades da Estratégia Saúde da Família. O estudo obteve aprovação do projeto de pesquisa pelo Comitê de Ética da Universidade Federal de Alagoas. Para a coleta dos dados utilizou-se instrumento testado, entrevista, exame físico e informações dos prontuários. Os dados foram organizados em planilha do Microsoft Excel 2007, exportados e analisados em software estatístico por meio de estatística descritiva e inferencial, considerando nível de significância estatística de ρ-valor < 0,05. As pessoas com úlcera venosa eram do sexo feminino (71,2%), ≥ 60 anos (67,8%) e estavam em tratamento > 1 ano (69,5%). Possuíam tempo de lesão > 6 meses (64,4%), dor na úlcera/membro (86,4%) e leito com ≤ 30% de granulação/epitelização (78,0%). A qualidade da assistência foi ruim (< 5 aspectos positivos) em 57,6% (ρ=0,000) e os aspectos que mais interferiram foram as seguintes inadequações: profissional que acompanha/realiza curativo (ρ=0,002, coeficiente de contingência (CC) =0,458, razão de chance (RC) =13,9), produtos nos últimos 30 dias (ρ=0,038, cc=0,334, RC=7,3) e acesso a consulta com angiologista (ρ=0,041, cc=0,305, RC=4,1). Os aspectos clínicos que contribuíram para o aumento do tempo de assistência foram: tempo de lesão >6 meses (ρ<0,001), dor (ρ=0,043), recidiva (ρ<0,001); nos aspectos assistenciais: inadequação dos produtos com 83,1% (ρ=0,036). Essas características dificultaram a cicatrização tecidual, prolongando o tempo de tratamento das lesões,que podem ter contribuído para a cronicidade das úlceras

Nanosistemas de penicilina G benzatina para tratamento profilático da febre reumática: estudo analítico

Investigations in the field of pharmaceutical analysis and quality control of medicines require analytical procedures with good perfomance characteristics. Calibration is one of the most important steps in chemical analysis, presenting direct relation to parameters such as linearity. This work consisted in the development of a new methodology to obtain calibration curves for drug analysis: the stationary cuvette one. It was compared to the currently used methodology, and possible sources of variation between them were evaluated. The results demonstrated that the proposed technique presented similar reproducibility compared to the traditional methodology. In addition to that, some advantages were observed, such as user-friendliness, cost-effectiveness, accuracy, precision and robustness. Therefore, the stationary cuvette methodology may be considered the best choice to obtain calibration curves for drug analyis by spectrophotometry

Otimização de solução extrativa e desenvolvimento tecnológico de produto seco por aspersão de Psidium guajava L.

The increasing in the consumption of plant medicine by parts of the population generated a bigger need for studies. Drug substitutions, changes and adulterations at the production techniques are common places at plant-originated drugs trade, leading governmental departments of drug control round the world to adopt many analytical practices to medicinal plants. However, agronomic and technological issues cause characteristics and chemical composition variation at the drug, problem to be solved by the subject researchers. The present work aims to obtain a spray dried extract from a extractive solution obtained from Psidium guajava L. leaves based in book references that stress the intermediate dosage forms advantages. It also tries to validate useful methodologies for the quality control for both raw material and its derivates. Using eight sets of the spray dried extract (with Eudragit®, Aerosil ® e Avicel PH101 ® as drying adjuvants), the study proposes analytical methods using techniques commonly performed to plant medicines and its intermediate forms. As results, a viable spray-dried extract was obtained from a standartized extract solution. Among the studied adjuvants, the combination Aerosil ® with Eudragit ® showed the drying outcome, rheology, humidity and tannin content values that best fitted the demands of the Brazilian Pharmacopaea

Desenvolvimento e validação de método analítico para determinação de teor de ácido gálico e catequina no fitoterápico sanativo® por cromatografia líquida de alta eficiência

The herbal medicine Sanativo® is produced by the Pernambucano Laboratory since 1888 with indications of healing and hemostasis. It is composed of a fluid extract about Piptadenia colubrina, Schinus terebinthifolius, Cereus peruvianus and Physalis angulata. Among the plants in their composition, S. terebinthifolius and P. colubrina have in common phenolic compounds which are assigned most of its pharmacological effects. The tannins, gallic acid and catechin were selected as markers for quality control. The aim of this study was the development and validation of analytical method by HPLC/UV/DAD for the separation and simultaneous quantification of gallic acid (GAC) and catechin (CTQ) in Sanativo®. The chromatographic system was to stationary phase, C-18 RP column, 4,6 x 150 mm (5 mm) under a temperature of 35 ° C, detection at 270 and 210 nm. The mobile phase consisted of 0.05% trifluoroacetic acid and methanol in the proportions 88:12 (v/v), a flow rate of 1 ml/min. The analytical method presented a retention factor of 0.30 and 1.36, tail factor of 1.8 and 1.63 for gallic acid and catechin, respectively, resolution of 18.2, and theoretical plates above 2000. The method validation parameters met the requirements of Resolution n º 899 of May 29, 2003, ANVISA. The correlation coefficient of linear regression analysis for GAC and CTQ from the standard solution was 0.9958 and 0.9973 and when performed from the Sanativo® 0.9973 and 0.9936, the matrix does not interfere in the range 70 to 110 %. The limits of detection and quantification for GAC and CQT were 3.25 and 0.863, and 9.57 and 2.55 mg/mL, respectively. The markers, GAC and CQT, showed repetibility (coefficient of variation of 0.94 % and 2.36 %) and satisfactory recovery (100.02 ± 1.11 % and 101.32 ± 1.36 %). The method has been characterized selective and robust quantification of GAC and CTQ in the Sanativo® and was considered validated

Desenvolvimento e validação de método analítico para determinação de WE010, WE014 e WE017

The synthetic guanylhydrazones WE010 (3,5-di-tert-butil-4-hidroxibenzaldehyde-guanylhydrazone), WE014 (4-bifenilcarboxialdehydeguanylhydrazone) and WE017 (3,4-diclorobenzaldehydeguanylhydrazone) showed high cytotoxic activity in terms of percentage inhibition of cancer cells growth. However, further progress in the development of these drug candidates requires precise and convenient methods for their qualitative and quantitative analyses. The aim of this study was to develop and validate High Performance Liquid Chromatography with diode-array detection (HPLC-DAD) and Ultra Fast Liquid Chromatography with diode-array detection (UFLC-DAD) methods suitable for as simultaneous as isolated determination of studied guanylhydrazones, based on the optimization of chromatographic parameters and obtaining reduced detection times. The chromatographic analyses of analytes by HPLC were performed on C18 ACE analytical column (150 mm x 4.6 mm), with a particle size of 5.0 μm. Among all the conditions assayed, the best results of separation were obtained with a mixture of methanol:water (60:40, v/v) as the mobile phase at a flow rate 1.5mL/min and pH of 3.5 adjusted at acetic acid. The UFLC method was developed by experimetal desing techniques in order to find optimal chromatographic analytical conditions, which were achieved on XR-ODS analytical column (50 mm x 3.0 mm), with a particle size of 2,2 μm, maintained at 25 ºC. The mobile phase was consisted of methanol:water (65:35, v/v) with 0.1% triethylamine (TEA) and pH of 3.5 adjusted at acetic acid, at a flow rate 0.5 mL/min. The procedure were validated following evaluating parameters such as specificity, linearity, limits of detection (LD) and quantification (LQ), precision, accuracy and robustness, giving results within the acceptable range. Although the UFLC method shows better sensitivity (lower values of LD and LQ), robustness (lower rates of relative standard deviation) and minimize spending time and solvent, both developed methods were adequately applied to the analysis of guanylhydrazones molecules, may be used in routine of quality control laboratories. Keywords: guanylhydrazones, HPLC/DAD, UFLC/DAD, validation of analitical method

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

A utilização do controle estatístico do processo para o monitoramento do sangue: estudo de caso no Memonorte-RN

The present work is grounded basically on the use of the Basic Tools for the Statistic Process Control SPC, with the intent to detect non-conformities on a given productive process. It consists on a case study accomplished at a Hemocenter in Natal (Rio Grande do Norte). In this study it is shown that, the Statistic Process Control Technique, which was used as a tool, is useful to identify on-conformities on the volume of hemocomponents. The gathering of the used data was performed by means of document analysis, direct observations and database queries. The results achieved from the study show that the analyzed products, even though when they have presented, in some cases, points out of control, they satisfied the ANVISA standards. Finally, suggestions for further improvement of the final product and guidance for future employment of CEP, also extended to other lines of production, are presented

Controle sanitário e ambiental de um projeto de reúso em um complexo de prédios corporativos

The study that resulted in this dissertation was developed at OU RNCE PETROBRAS, in Natal, which implemented a project of rational use and reuse of water, including use of wastewater from a Sewage Treatment Plant (STP) already in place, diluted with water from own wells for irrigation of green area of the building complex corporate enterprise. Establish a methodology that can serve as guidelines for future projects controlled reuse of water like this was the objective of this research. Been proposed, implemented and evaluated three instruments of sanitary and environmental control: 1) adaptation of sewage treatment plant and quality control of the treated effluent 2) analysis of soil-nutrient interaction in the irrigated area, 3) knowledge of the local hydrogeology, especially with regard to the direction of flow of the aquifer and location of collection wells of Companhia de Águas e Esgotos do Rio Grande do Norte (CAERN) situated in the surroundings. These instruments have proven sufficient and appropriate to ensure the levels of sanitary and environmental control proposed and studied, which were: a) control of water quality off the STP and the output of the irrigation reservoir, b) control of water quality sub surface soil and assessment of progress on soil composition, c) assessment of water quality in the aquifer. For this, we must: 1) establishing the monitoring plan of the STP and its effluent quality sampling points and defining the parameters of analysis, improve the functioning of that identifying the adequacy of flow and screening as the main factors of operational control, and increase the efficiency of the station to a relatively low cost, using additional filters, 2) propose, implement and adapt simple collectors to assess the quality of water percolating into the soil of the irrigated area, 3) determine the direction of groundwater flow in the area study and select the wells for monitoring of the aquifer.

Análises físico-químicas de polpas de frutas e avaliação dos seus padrões de identidade e qualidade

The pulps are products that add economic value enjoy the fruits of the surplus productions of the same. Have good market acceptance because of its practicality and diversity of flavors available year round. In order to assess the quality of the fruit pulp through the physical and chemical parameters and the characteristics of manufacturing industry, we analyzed 36 samples of frozen fruit pulp of three brands marketed in RIO Grande do Norte, 14 brand A, 12 of 10 brand B and brand C, which corresponded to 14 different flavors, of which 10 have identity Standards and Quality (ISQ S) established by the Ministério da Agricultura, Pecuária e Abastecimento (MAPA), totaling 27 samples with ISQ s. We conducted the following physicalchemical analyzes on samples of fruit pulp: Total solids, total soluble solids, pH, titratable acidity, total sugars and the determination of ascorbic acid. The percentage of failure for each parameter evaluated was 37, 04% in total soluble solids, 22,22% for total solids and titratable acidity, 7,40% in relation to pH. The total sugars were within the requirements demanded by the MAPA and ascorbic acid content, determined only in the pulp of acerola and cashew, presented a non compliance in the pulp of brand B. The percentage of failures of the pulps with ISQ S was 59% with brand A, B and C accounted for 3,70%, 33,33% and 22,22% respectively. The pulps which have no established atandards such as pineapple pulp, showed similar values between brands and literature data unlike the pulp of plum, jackfruit and tamarind which diverged greatly in parameters such as total solids and total soluble solids. The study demonstrates the need for greater quality control by the producers with respect to raw materials, processing, packing, stored and the importance of ISQ S to establish the flavors have not yet covered by existing legislation, but already highly commercialized

Beta: uma ferramenta para geração de testes de unidade a partir de especificações B

Formal methods and software testing are tools to obtain and control software quality. When used together, they provide mechanisms for software specification, verification and error detection. Even though formal methods allow software to be mathematically verified, they are not enough to assure that a system is free of faults, thus, software testing techniques are necessary to complement the process of verification and validation of a system. Model Based Testing techniques allow tests to be generated from other software artifacts such as specifications and abstract models. Using formal specifications as basis for test creation, we can generate better quality tests, because these specifications are usually precise and free of ambiguity. Fernanda Souza (2009) proposed a method to define test cases from B Method specifications. This method used information from the machine s invariant and the operation s precondition to define positive and negative test cases for an operation, using equivalent class partitioning and boundary value analysis based techniques. However, the method proposed in 2009 was not automated and had conceptual deficiencies like, for instance, it did not fit in a well defined coverage criteria classification. We started our work with a case study that applied the method in an example of B specification from the industry. Based in this case study we ve obtained subsidies to improve it. In our work we evolved the proposed method, rewriting it and adding characteristics to make it compatible with a test classification used by the community. We also improved the method to support specifications structured in different components, to use information from the operation s behavior on the test case generation process and to use new coverage criterias. Besides, we have implemented a tool to automate the method and we have submitted it to more complex case studies

Evolving Future Internet clean-slate Entity Title Architecture with quality-oriented control-plane extensions

A Internet atual vem sofrendo vários problemas em termos de escalabilidade, desempenho, mobilidade, etc., devido ao vertiginoso incremento no número de usuários e o surgimento de novos serviços com novas demandas, propiciando assim o nascimento da Internet do Futuro. Novas propostas sobre redes orientadas a conteúdo, como a arquitetura Entidade Titulo (ETArch), proveem novos serviços para este tipo de cenários, implementados sobre o paradigma de redes definidas por software. Contudo, o modelo de transporte do ETArch é equivalente ao modelo best-effort da Internet atual, e vem limitando a confiabilidade das suas comunicações. Neste trabalho, ETArch é redesenhado seguindo o paradigma do sobreaprovisionamento de recursos para conseguir uma alocação de recursos avançada integrada com OpenFlow. Como resultado, o framework SMART (Suporte de Sessões Móveis com Alta Demanda de Recursos de Transporte), permite que a rede defina semanticamente os requisitos qualitativos das sessões para assim gerenciar o controle de Qualidade de Serviço visando manter a melhor Qualidade de Experiência possível. A avaliação do planos de dados e de controle teve lugar na plataforma de testes na ilha do projeto OFELIA, mostrando o suporte de aplicações móveis multimídia com alta demanda de recursos de transporte com QoS e QoE garantidos através de um esquema de sinalização restrito em comparação com o ETArch legado

Avaliação da aplicabilidade de correlações matemáticas e redes neurais na predição de parâmetros de especificação do diesel

Diesel fuel is one of leading petroleum products marketed in Brazil, and has its quality monitored by specialized laboratories linked to the National Agency of Petroleum, Natural Gas and Biofuels - ANP. The main trial evaluating physicochemical properties of diesel are listed in the resolutions ANP Nº 65 of December 9th, 2011 and Nº 45 of December 20th, 2012 that determine the specification limits for each parameter and methodologies of analysis that should be adopted. However the methods used although quite consolidated, require dedicated equipment with high cost of acquisition and maintenance, as well as technical expertise for completion of these trials. Studies for development of more rapid alternative methods and lower cost have been the focus of many researchers. In this same perspective, this work conducted an assessment of the applicability of existing specialized literature on mathematical equations and artificial neural networks (ANN) for the determination of parameters of specification diesel fuel. 162 samples of diesel with a maximum sulfur content of 50, 500 and 1800 ppm, which were analyzed in a specialized laboratory using ASTM methods recommended by the ANP, with a total of 810 trials were used for this study. Experimental results atmospheric distillation (ASTM D86), and density (ASTM D4052) of diesel samples were used as basic input variables to the equations evaluated. The RNAs were applied to predict the flash point, cetane number and sulfur content (S50, S500, S1800), in which were tested network architectures feed-forward backpropagation and generalized regression varying the parameters of the matrix input in order to determine the set of variables and the best type of network for the prediction of variables of interest. The results obtained by the equations and RNAs were compared with experimental results using the nonparametric Wilcoxon test and Student's t test, at a significance level of 5%, as well as the coefficient of determination and percentage error, an error which was obtained 27, 61% for the flash point using a specific equation. The cetane number was obtained by three equations, and both showed good correlation coefficients, especially equation based on aniline point, with the lowest error of 0,816%. ANNs for predicting the flash point and the index cetane showed quite superior results to those observed with the mathematical equations, respectively, with errors of 2,55% and 0,23%. Among the samples with different sulfur contents, the RNAs were better able to predict the S1800 with error of 1,557%. Generally, networks of the type feedforward proved superior to generalized regression.

Desenvolvimento de metodologias analíticas alternativas por cromatografia gasosa para análise de biodiesel

Since the beginning of the National Program for Production and Use of Biodiesel in Brazil, in 2004, different raw materials were evaluated for biodiesel production, trying to combine the agricultural diversity of the country to the desire to reduce production coasts. To determine the chemical composition of biodiesel produced from common vegetables oils, international methods have been used widely in Brazil. However, for analyzing biodiesel samples produced from some alternative raw materials analytical problems have been detected. That was the case of biodiesel from castor oil. Due the need to overcome these problems, new methodologies were developed using different chromatographic columns, standards and quantitative methods. The priority was simplifying the equipment configuration, realizing faster analyses, reducing the costs and facilitating the routine of biodiesel research and production laboratories. For quantifying free glycerin, the ethylene glycol was used in instead of 1,2,4-butanetriol, without loss of quality results. The ethylene glycol is a cheaper and easier standard. For methanol analyses the headspace was not used and the cost of the equipment used was lower. A detailed determination of the esters helped the deeper knowledge of the biodiesel composition. The report of the experiments and conclusions of the research that resulted in the development of alternative methods for quality control of the composition of the biodiesel produced in Brazil, a country with considerable variability of species in agriculture, are the goals of this thesis and are reported in the following pages