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

Caracterização e quantificação de marcadores químicos do extrato hidroetanólico das folhas de Kalanchoe brasiliensis Cambess

Kalanchoe brasiliensis Cambess (Crassulaceae), commonly known as saião , coirama branca , folha grossa , is originally from Brazil and commonly found in São Paulo to Bahia, mainly in the coastal zone. Regarding of biological activities, most preclinical studies were found in the literature, mainly about the anti-inflammatory activity of extracts obtained from leaves and / or aerial parts of K. brasiliensis. As regards the chemical constitution, it has been reported mainly the presence of flavonoids in the leaves of the species, but until this moment did not knows which are the active compounds. Although it is a species widely used in traditional medicine in Brazil, there is no monograph about the quality parameters of the plant drug. In this context, this study aims to characterize and quantify the chemical markers of hydroethanolic extract (HE) from the leaves of K. brasiliensis, which can be used in quality control of plant drug and derivatives obtained from this species. The methodology was divided into two parts: i. Phytochemical study: to fractionate, isolate and characterizate of the chemical (s) marker (s) of the HE from the leaves of K. brasiliensis; ii. To Developed validate of analytical method by High Performance Liquid Chromatography (HPLC)-diode array detector (DAD) to quantify the chemical (s) marker (s) of the EH. i. The EH 50% was prepared by turbo extraction method. It was then submitted to liquid-liquid partition, obtaining dichloromethane, n-butanol and ethyl acetate (AcOEt) fractions. The AcOEt fraction was selected to continue the fractionation process, because it has a chemical profile rich in flavonoids. The acOEt fraction was submitted to column chromatography using different systems for obtaining the compound Kb1. To identify this compound, it was submitted to UV analysis ii. For quantitative analysis, the EH was analyzed by HPLC, using different methods. After selecting the most appropriate method, which showed satisfactory resolution and symmetrical peaks, it was validated according to parameters in the RE 899/2003. As result, it was obtained from the AcOEt fraction the compound Kb1 (2.7 mg). Until this moment, the basic nucleus was characterized by UV analysis using shift reagents. The partial chemical structure of the compound Kb1 was identified as a flavonol, containing hydroxyls in 3 , 4 position (ring A), 5 and 7 free (ring B) and a replacement of the C3 hydroxyl by a sugar. As the analysis were performed in the HPLC coupled to a DAD, we observed that the UV spectrum of the major peaks of EH from K. brasiliensis shown similar UV spectrum. According to the literature, it has been reported the presence of patuletin glycosydes derivatives in the leaves of this species. Therefore, it is suggested that the compound Kb1 is glycosylated patuletin derivative. Probably the sugar (s) unit(s) are linked in the C3 in the C ring. . Regarding the development of HPLC analytical method, the system used consists of phase A: water: formic acid (99,7:0,3, v / v) and phase B: methanol: formic acid (99,7:0,3, v / v), elution gradient of 40% B - 58% B in 50 minutes, ccolumn (Hichrom ®) C18 (250x4, 0 mm, 5 μm), flow rate 0.8 mL / min, UV detection at 370 nm, temperature 25 ° C. In the analysis performed with the co-injection of thecompound Kb1 + HE of K. brasiliensis was observed that it is one of the major compounds with a retention time of 12.47 minutes and had a content of 15.3% in EH of leaves from K. brasiliensis. The method proved to be linear, precise, accurate and reproducible. According to these results, it was observed that compound Kb1 can be used as a chemical marker of EH from leaves of K. brasiliensis, to assist in quality control of drug plant and its derivatives

Avaliação in vitro da eficácia de produtos homeopáticos contendo momordica charantia através de bioensaios

Homeopathic medicines have been used for over two hundred years without the examination of their effects on in vivo and in vitro assays, due to the peculiarity of homeopathic preparations, the high dilution, which creates a challenge for the use of usual analytical techniques of quality control of medicine.Although there is scarcity of literature and variety of experiments, recently there have been some studies with few in vitro assays which have shown positive responses when evaluating the mechanism of action of homeopathic medicines which are able to act on a specific system.The present study aims to evaluate the efficacy of homeopathic products containing Momordica charantia through bioassays.Homeopathic products were tested by the MTT to assess cytotoxicity in RAW 264.7 (macrophage-like cells) and in tumor cells HeLa (human cervical adenocarcinoma cells), CHO K1 (Chinese hamster ovary cells), PANC-1 (human pancreas cancer cells) and PC-3 (human prostate cancer cells), dosage of inflammatory mediators NO, TNF-α and IL-6 released by RAW 264.7 cells, analysis of the death process and cell cycle changes of PC-3 by flow cytometry. The data demonstrate that homeopathic products of Momordica charantia did not show cytotoxicity to RAW 264.7, increased the production of inflammatory mediators by RAW 264.7 synergistically with LPS, showed cytotoxicity to PC-3 with change in its cell cycle inhibiting its proliferation, being the 30CH the most potent sample. Correlation studies were conducted in order to evaluate the possible in vitro applicable models to the quality control of homeopathic products with Momordica charantia. The data showed that the best applicable models in assessing the quality are the MTT to assess cytotoxicity in RAW 264.7 and PC-3 in 24 hours for Momordica charantia fruit products and dosage of NO production by RAW 264.7 with and without LPS

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

Testes bioquímicos para avaliação do vigor em sementes de Mimosa caesalpiniaefolia Benth

Mimosa caesalpiniaefolia Benth. is a forest species of the Mimosaceae family, recommended for recovery of degraded areas. The evaluation of vigor by biochemical tests have been an important tool in the control of seed quality programs, and the electrical conductivity and potassium leaching the most efficient in the verifying the physiological potential. The objective, therefore, to adjust the methodology of the electrical conductivity test for seeds of M. caesalpiniaefolia, for then compare the efficiency of this test with the potassium in the evaluation of seed vigor of different lots of seeds M. caesalpiniaefolia. To test the adequacy of the electrical conductivity were used different combinations of temperatures , 25 °C and 30 ºC, number of seeds , 25 and 50, periods of imbibition , 4 , 8 , 12 , 16 and 24 hours , and volumes deionized water, 50 mL and 75mL. For potassium leaching test, which was conducted from the results achieved by the methodology of the adequacy of the electrical conductivity test, to compare the efficiency of both tests , in the classification of seeds at different levels of vigor, and the period 4 hours also evaluated because the potassium leaching test can be more efficient in the shortest time . The best combination obtained in experiment of electrical conductivity is 25 seeds soaked in 50 mL deionized or distilled water for 8 hours at a temperature of 30 ° C. Data were subjected to analysis of variance, the means were compared with each other by F tests and Tukey at 5 % probability, and when necessary polynomial regression analysis was performed. The electrical conductivity test performed at period eight hour proved to be more efficient in the separation of seed lots M. caesalpiniaefolia at different levels of vigor compared to the potassium test

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

Sistema Híbrido de Inferência Baseado em Análise de Componentes Principais e Redes Neurais Artificiais Aplicado a Plantas de Processamento de Gás Natural

Nowadays, where the market competition requires products with better quality and a constant search for cost savings and a better use of raw materials, the research for more efficient control strategies becomes vital. In Natural Gas Processin Units (NGPUs), as in the most chemical processes, the quality control is accomplished through their products composition. However, the chemical composition analysis has a long measurement time, even when performed by instruments such as gas chromatographs. This fact hinders the development of control strategies to provide a better process yield. The natural gas processing is one of the most important activities in the petroleum industry. The main economic product of a NGPU is the liquefied petroleum gas (LPG). The LPG is ideally composed by propane and butane, however, in practice, its composition has some contaminants, such as ethane and pentane. In this work is proposed an inferential system using neural networks to estimate the ethane and pentane mole fractions in LPG and the propane mole fraction in residual gas. The goal is to provide the values of these estimated variables in every minute using a single multilayer neural network, making it possibly to apply inferential control techniques in order to monitor the LPG quality and to reduce the propane loss in the process. To develop this work a NGPU was simulated in HYSYS R software, composed by two distillation collumns: deethanizer and debutanizer. The inference is performed through the process variables of the PID controllers present in the instrumentation of these columns. To reduce the complexity of the inferential neural network is used the statistical technique of principal component analysis to decrease the number of network inputs, thus forming a hybrid inferential system. It is also proposed in this work a simple strategy to correct the inferential system in real-time, based on measurements of the chromatographs which may exist in process under study

Adaptação de um sistema automatizado para medição de microdureza

The hardness test is thoroughly used in research and evaluation of materials for quality control. However, this test results are subject to uncertainties caused by the process operator in the moment of the mensuration impression diagonals make by the indenter in the sample. With this mind, an automated equipment of hardness mensuration was developed. The hardness value was obtained starting from the mensuration of plastic deformation suffered by the material to a well-known load. The material deformation was calculated through the mensuration of the difference between the progress and retreat of a diamond indenter on the used sample. It was not necessary, therefore, the manual mensuration of the diagonals, decreasing the mistake source caused by the operator. Tension graphs of versus deformation could be analyzed from data obtained by the accomplished analysis, as well as you became possible a complete observation of the whole process. Following, the hardness results calculated by the experimental apparatus were compared with the results calculated by a commercial microhardness machine with the intention of testing its efficiency. All things considered, it became possible the materials hardness mensuration through an automated method, which minimized the mistakes caused by the operator and increased the analysis reliability

A engenharia simultânea e o perfil da indústria de confecção da grande Natal/RN utilizando as ferramentas CAD/PDM e ERP

This work presents the research carried through in the industrial segment of confection of clothes of the Great Natal whose objective is to show the profile, enterprise and technological management as also the use of simultaneous engineering in the development of products. The research approaches two studies. The first one presents the current picture of the companies, synthesized through twelve variable. As, through fifteen variable it shows to the level of use of Simultaneous Engineering in the Development of Products and its amplitude in relation to the Integrated Management using tools CAD, PDM and ERP (Computer Aided Design, Product Management Date, Enterprise Resource Planning). The integration of these systems acts aiming the reduction of the cost and the development time of products. The reached results indicate that simultaneous engineering is a competitive advantage and becomes possible: to reduce the life cycle of the product, to rationalize the resources, to incorporate one high standard of the quality to the process and product as well as to personalize the product to take care of the global market. It is important to note that this work also is considered to contribute for the better understanding of the real companies situation of confection located at the Great Natal and its role in the economy of the State of the Rio Grande do Norte

Caracterização e avaliação do macro sistema urbano de distribuição de água de Natal RN

The aim of this study is to characterize and evaluate the Macro System of Regional Water Distribution Natal North (RNN) and Southern Regional Natal (RNS), covering 35% and 65% respectively of the Natal-RN City. The terms of the quality and quantity of water (surface and groundwater) were also evaluated in order to adjust the parameters that contribute to proper distribution and control in water reserves. The methodology of the work took place from collecting volumetric data of production capacity and distribution of the two treatment plants for Regional as well as the flow rates of wells. Yet the quantitative capacity of reservation, distribution and consumption of the main reservoirs, population numbers and consumption of members neighborhoods were collected. Data were tabulated and used in computational simulator EPANET to diagnose possible through the water balance, the offers and demands on the water supply system in the neighborhoods of the capital, linking them to specific distribution points. We also evaluated the wells in the levels of nitrate in water consumed. As a result it was found that some neighborhoods in the South Regional Natal, was ranked as critical supply situation: City of Hope, Lagoa Nova and Nova Descoberta, where demand exceeds supply. While in most Northern Regional Natal present deficiency in the supply system as: Lagoa Azul, the Parque dos Coqueiros, igapó, Amarante and Salinas. The rates of nitrate in the city were significant, but manageable with corrective and preventive measures. The averages were 12 mg /l-N in Candelária, 10 mg/l-N in Lagoa Nova, 9 mg/l-N in Satelite, 20 mg/l-N in Gramore and 15 mg/l-N in N. Sra. Apresentação. Therefore proper distribution of water abstracted and implementation of quality control ensures the supply required by the system, associated with preservation of Water Resources of the Metropolitan Region of Natal

Estudo termoanalítico de medicamentos de referência, genérico e similar

This study aimed to apply, thermogravimetriy /derivative Thermogravimetriy (TG/DTG), differential scanning calorimetry (DSC), Differential Thermal Analysis (DTA), to conduct a comparative study on drug reference, generic and whose active principles are similar captopril hydrochlorothiazide, ampicillin, paracetamol, aspirin and mebendazole sold in local pharmacies. Samples of the active ingredients and dosage forms were also characterized by absorption infrared spectroscopy (IR), X-ray diffraction (XRD) and microscopy scanning electron (SEM). The TG / DTG curves showed a general similarity in the thermal behavior of the samples, but also showed the influence of excipients on the thermal stability. The DSC curve of the generic base hydrochlorothiazide showed no peak on the fusion of the drug due to interference of lactose as a diluent, which causes interaction with the active principle causing their degradation before the merger. The DSC curves of the drugs consisting of paracetamol showed reproducibility at the melting point of the active and the other thermal events. The DSC result of binary mixtures involving captopril / magnesium stearate and mebendazole/magnesium stearate showed possible interactions or incompatibilities evidenced by the displacement of the melting point of both drugs. The other mixtures showed no change. The infrared spectra presented were very similar, indicating the presence of functional groups characteristic of the constituents of the samples. The X-ray diffraction showed peaks indicative of crystalline structure of the active ingredients as well as some of the ingredients in the formulation of the drug and the micrographs indicate a general heterogeneity in the size distribution of particles in the samples

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