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

Otimização evalidação de métodos analíticos para a determinação simultânea de tuberculostáticos (4-FDC) por CLAE/DAD e CLUE/ DAD

Tuberculosis is a serious disease, but curable in practically 100% of new cases, since complied the principles of modern chemotherapy. Isoniazid (ISN), Rifampicin (RIF), Pyrazinamide (PYR) and Chloride Ethambutol (ETA) are considered first line drugs in the treatment of tuberculosis, by combining the highest level of efficiency with acceptable degree of toxicity. Concerning USP 33 - NF28 (2010) the chromatography analysis to 3 of 4 drugs (ISN, PYR and RIF) last in average 15 minutes and 10 minutes more to obtain the 4th drug (ETA) using a column and mobile phase mixture different, becoming its industrial application unfavorable. Thus, many studies have being carried out to minimize this problem. An alternative would use the UFLC, which is based with the same principles of HPLC, however it uses stationary phases with particles smaller than 2 μm. Therefore, this study goals to develop and validate new analytical methods to determine simultaneously the drugs by HPLC/DAD and UFLC/DAD. For this, a analytical screening was carried out, which verified that is necessary a gradient of mobile phase system A (acetate buffer:methanol 94:6 v/v) and B (acetate buffer:acetonitrile 55:45 v/v). Furthermore, to the development and optimization of the method in HPLC and UFLC, with achievement of the values of system suitability into the criteria limits required for both techniques, the validations have began. Standard solutions and tablets test solutions were prepared and injected into HPLC and UFLC, containing 0.008 mg/mL ISN, 0.043 mg/mL PYR, 0.030 mg.mL-1 ETA and 0.016 mg/mL RIF. The validation of analytical methods for HPLC and UFLC was carried out with the determination of specificity/selectivity, analytical curve, linearity, precision, limits of detection and quantification, accuracy and robustness. The methods were adequate for determination of 4 drugs separately without interfered with the others. Precise, due to the fact of the methods demonstrated since with the days variation, besides the repeatability, the values were into the level required by the regular agency. Linear (R> 0,99), once the methods were capable to demonstrate results directly proportional to the concentration of the analyte sample, within of specified range. Accurate, once the methods were capable to present values of variation coefficient and recovery percentage into the required limits (98 to 102%). The methods showed LOD and LOQ very low showing the high sensitivity of the methods for the four drugs. The robustness of the methods were evaluate, facing the temperature and flow changes, where they showed robustness just with the preview conditions established of temperature and flow, abrupt changes may influence with the results of methods

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

Do mestre aos discípulos: o legado educacional de Nestor dos Santos Lima (1910-1930)

Cette étude analyse La pratique pédagogique de l éducateur norte-rio-grandense Nestor dos Santos Lima, de 1910 a 1930, période ou se concentre son plus grand nombre de publications sur lês questions scolaires. Nous désirons comprendre de quelle forme cet intelectuel a contribué au développement du systeème d enseignement primaire à travers sés écrits sur lês principes et méthodes de l enseignement de la lecture et à l écriture, appliqués dans lês Groupes Scolaires de l État. Nestor Lima a joué um grand role dans la sociaété, à la tetê de fonctoins comme celle de La présidence de l Institut Historique e Geographique du Rio Grande do Norte (IHGRN), directeur de lÉcole Normale de Natal et du Dápartament d Education de État. Il a pulié de diverses oeuvres de caractere scolaire, comme lês Régiments Internes pour lês Groupes Scolaires, Écoles Isolées, Écoles Rudimentaires et Conseil d Education. Dans cette étude, nous mettons em évidence lês leçons de métodologique pour l enseignement de la lecture ET de évidence lês leçons de metodologie pour l enseignement de la lecture et de l ecriture, adresses aus eleves de lÉcole Normale de Natal, publiées dans la colonne Pádagogie du journal A República. Dans ces matièrs, nous observons que lês aspects qui composaient la pratique développe par Nestor Lima impliquaient lês questions Morales et civiques, la preocupation de la formation enseignante à l École Normale de Natal et le Célibat Pédagogique Féminin. Nous observons que la preocupations dês pratiques de lecture et lécriture sont presentes dans l oeuvre de cet éducateur comme legs important aux générations qui se succédent. Il est évident qu Il a cherché das sés productions une meilleure qualification dês enseignants pour que le niveau de l enseignement primaire puísse ainsi évoluer

Concepções de policiais militares sobre cuidados com a saúde

A ausência de cuidados do homem com a saúde representa um fenômeno significativo, pois contribui para o aumento da morbidade e mortalidade masculina por causas evitáveis. Essa realidade torna-se mais relevante quando se trata do policial militar, devido às peculiaridades do seu processo de trabalho. Visto isso, considera-se que os cuidados de saúde adotados por policiais militares atrelam-se ao entendimento de que possuem sobre os agravos à saúde, o qual perpassa por concepções de gênero e da profissão. Isso levou ao seguinte questionamento: Como o policial militar concebe os cuidados com a saúde. Objetivou-se analisar concepções de policiais militares sobre cuidados com a saúde. Trata-se de um estudo exploratório e descritivo, com abordagem qualitativa, desenvolvido junto a um Batalhão Militar do Comando de Policiamento de Natal, Rio Grande do Norte, Brasil. A coleta de dados foi realizada no período de junho a julho de 2013. Essa etapa foi antecedida pela anuência do Comandante Geral da Polícia Militar do Rio Grande do Norte, sob a aprovação do Comitê de Ética em Pesquisa da Universidade Federal do Rio Grande do Norte, com o CAAE nº 15449713.7.0000.5537, e autorização formal dos entrevistados mediante a assinatura do Termo de Consentimento Livre e Esclarecido (TCLE), atendendo às exigências da Resolução 466/2012, do Conselho Nacional de Saúde, no que se refere à pesquisa com seres humanos. Participaram do estudo 21 policiais militares, do sexo masculino, que trabalhavam no policiamento ostensivo, não estavam de licença médica e apresentaram condições psicológicas e/ou físicas favoráveis para responder aos questionamentos. Os dados foram coletados por meio de entrevista semiestruturada mediante um roteiro constituído de duas partes: a primeira com questões sociodemográficas com vistas à caracterização dos participantes da pesquisa e a segunda com duas questões norteadoras relativas ao objeto de estudo. Os depoimentos foram tratados conforme o método de análise de conteúdo na modalidade de análise temática segundo Bardin. Desse processo, emergiram três categorias: hábitos de vida de policiais militares, repercussão do trabalho na saúde de policiais militares e atitudes de policiais militares em frente dos problemas de saúde. A análise dos dados foi subsidiada pelo referencial teórico do Modelo de Crenças em Saúde (Health Belief Model), de acordo com as variáveis vulnerabilidade e barreiras . Para respaldar a discussão dos resultados, buscou-se na literatura conhecimentos acerca da saúde do homem e do policial militar. Os resultados apontaram que os entrevistados procuram cuidar da saúde com práticas de exercícios físicos, alimentos saudáveis e preservação do sono. No entanto, vivenciam dores de coluna, ganho de peso, dificuldades para dormir, estresse e sofrimento psicológico. Diante disso, eles buscam apoio quando acometidos por agravos à saúde e reconhecem a necessidade de medidas de segurança durante o serviço. Portanto, notam a sua condição de vulnerabilidade em decorrência de seu ofício, porém enfrentam dificuldades na adoção de práticas preventivas de agravos a saúde. Mediante os resultados, faz-se necessário que o enfermeiro atuante junto a este público elabore, implemente e acompanhe estratégias de atenção a sua saúde

Oportunidades de melhoria ergonômica das exigências físicas da atividade jangadeira em Ponta Negra Natal-RN

The fishing is an activity with rafts marked by unpredictability, poor tools, physical stress, awkward postures, risk of accidents and incidents, which contribute to insecurity in the context of activity. This study aimed to contribute to reducing of physical effort and the biomechanical impacts in jangadeiro activity of artisanal fishing using jangadas on the beach of Ponta Negra, Natal-RN. To achieve this purpose the methodology of the Work Ergonomic Analysis - WEA became a reference using techniques such as observational and interactional observation notes, photographs, videos, action conversational and listening verbalizations. The resulting activity in health jangadeiro, discussed in this research were: static postural assessment, flexibility of movement of shoulder flexion-extension, flexibility of the hamstrings and lower back, grip and musculoskeletal pain. It was found from observations, interactions and activity analysis, that in carrying out fishing rafts are frequent awkward postures associated with demand for power and many are already feeling the jangadeiros reflections of years of life dedicated to this work. These have already adopted some measures to manage the activity, such as job rotation during the expedition of capture. Therefore, there is a need to expand these measures of activity management, as well as design and capabilities of the raft, seeking positive changes in the activity and consequently the quality of life jangadeiro

Estudo de estratégias de otimização para poços de petróleo com elevação por bombeio de cavidades progressivas

The progressing cavity pump artificial lift system, PCP, is a main lift system used in oil production industry. As this artificial lift application grows the knowledge of it s dynamics behavior, the application of automatic control and the developing of equipment selection design specialist systems are more useful. This work presents tools for dynamic analysis, control technics and a specialist system for selecting lift equipments for this artificial lift technology. The PCP artificial lift system consists of a progressing cavity pump installed downhole in the production tubing edge. The pump consists of two parts, a stator and a rotor, and is set in motion by the rotation of the rotor transmitted through a rod string installed in the tubing. The surface equipment generates and transmits the rotation to the rod string. First, is presented the developing of a complete mathematical dynamic model of PCP system. This model is simplified for use in several conditions, including steady state for sizing PCP equipments, like pump, rod string and drive head. This model is used to implement a computer simulator able to help in system analysis and to operates as a well with a controller and allows testing and developing of control algorithms. The next developing applies control technics to PCP system to optimize pumping velocity to achieve productivity and durability of downhole components. The mathematical model is linearized to apply conventional control technics including observability and controllability of the system and develop design rules for PI controller. Stability conditions are stated for operation point of the system. A fuzzy rule-based control system are developed from a PI controller using a inference machine based on Mandami operators. The fuzzy logic is applied to develop a specialist system that selects PCP equipments too. The developed technics to simulate and the linearized model was used in an actual well where a control system is installed. This control system consists of a pump intake pressure sensor, an industrial controller and a variable speed drive. The PI control was applied and fuzzy controller was applied to optimize simulated and actual well operation and the results was compared. The simulated and actual open loop response was compared to validate simulation. A case study was accomplished to validate equipment selection specialist system

Classificação de imagens de ambientes coralinos: uma abordagem empregando uma combinação de classificadores e máquina de vetor de suporte

The use of the maps obtained from remote sensing orbital images submitted to digital processing became fundamental to optimize conservation and monitoring actions of the coral reefs. However, the accuracy reached in the mapping of submerged areas is limited by variation of the water column that degrades the signal received by the orbital sensor and introduces errors in the final result of the classification. The limited capacity of the traditional methods based on conventional statistical techniques to solve the problems related to the inter-classes took the search of alternative strategies in the area of the Computational Intelligence. In this work an ensemble classifiers was built based on the combination of Support Vector Machines and Minimum Distance Classifier with the objective of classifying remotely sensed images of coral reefs ecosystem. The system is composed by three stages, through which the progressive refinement of the classification process happens. The patterns that received an ambiguous classification in a certain stage of the process were revalued in the subsequent stage. The prediction non ambiguous for all the data happened through the reduction or elimination of the false positive. The images were classified into five bottom-types: deep water; under-water corals; inter-tidal corals; algal and sandy bottom. The highest overall accuracy (89%) was obtained from SVM with polynomial kernel. The accuracy of the classified image was compared through the use of error matrix to the results obtained by the application of other classification methods based on a single classifier (neural network and the k-means algorithm). In the final, the comparison of results achieved demonstrated the potential of the ensemble classifiers as a tool of classification of images from submerged areas subject to the noise caused by atmospheric effects and the water column

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

Desenvolvimento de um simulador de bombeio por cavidades progressivas

The method of artificial lift of progressing cavity pump is very efficient in the production of oils with high viscosity and oils that carry a great amount of sand. This characteristic converted this lift method into the second most useful one in oil fields production. As it grows the number of its applications it also increases the necessity to dominate its work in a way to define it the best operational set point. To contribute to the knowledge of the operational method of artificial lift of progressing cavity pump, this work intends to develop a computational simulator for oil wells equipped with an artificial lift system. The computational simulator of the system will be able to represent its dynamic behavior when submitted to the various operational conditions. The system was divided into five subsystems: induction motor, multiphase flows into production tubing, rod string, progressing cavity pump and annular tubing-casing. The modeling and simulation of each subsystem permitted to evaluate the dynamic characteristics that defined the criteria connections. With the connections of the subsystems it was possible to obtain the dynamic characteristics of the most important arrays belonging to the system, such as: pressure discharge, pressure intake, pumping rate, rod string rotation and torque applied to polish string. The shown results added to a friendly graphical interface converted the PCP simulator in a great potential tool with a didactic characteristic in serving the technical capability for the system operators and also permitting the production engineering to achieve a more detail analysis of the dynamic operational oil wells equipped with the progressing cavity pump

Controle Robusto Aplicado a Conversor Buck-Boost em Sistemas Fotovoltaicos

The need to implement a software architecture that promotes the development of a SCADA supervisory system for monitoring industrial processes simulated with the flexibility of adding intelligent modules and devices such as CLP, according to the specifications of the problem, it was the motivation for this work. In the present study, we developed an intelligent supervisory system on a simulation of a distillation column modeled with Unisim. Furthermore, OLE Automation was used as communication between the supervisory and simulation software, which, with the use of the database, promoted an architecture both scalable and easy to maintain. Moreover, intelligent modules have been developed for preprocessing, data characteristics extraction, and variables inference. These modules were fundamentally based on the Encog software

Simulador computacional para poços de petróleo com método de elevação artificial por bombeio mecânico

This work proposes a computer simulator for sucker rod pumped vertical wells. The simulator is able to represent the dynamic behavior of the systems and the computation of several important parameters, allowing the easy visualization of several pertinent phenomena. The use of the simulator allows the execution of several tests at lower costs and shorter times, than real wells experiments. The simulation uses a model based on the dynamic behavior of the rod string. This dynamic model is represented by a second order partial differencial equation. Through this model, several common field situations can be verified. Moreover, the simulation includes 3D animations, facilitating the physical understanding of the process, due to a better visual interpretation of the phenomena. Another important characteristic is the emulation of the main sensors used in sucker rod pumping automation. The emulation of the sensors is implemented through a microcontrolled interface between the simulator and the industrial controllers. By means of this interface, the controllers interpret the simulator as a real well. A "fault module" was included in the simulator. This module incorporates the six more important faults found in sucker rod pumping. Therefore, the analysis and verification of these problems through the simulator, allows the user to identify such situations that otherwise could be observed only in the field. The simulation of these faults receives a different treatment due to the different boundary conditions imposed to the numeric solution of the problem. Possible applications of the simulator are: the design and analysis of wells, training of technicians and engineers, execution of tests in controllers and supervisory systems, and validation of control algorithms

Estudo da estimativa da incerteza de medição para determinação do BS&W e da vazão aplicado no laboratório de avaliação de medição do petróleo

The considered work presents the procedure for evaluation of the uncertainty related to the calibration of flow measurers and to BS&W. It is about a new method of measurement purposed by the conceptual project of the laboratory LAMP, at Universidade Federal do Rio Grande do Norte, that intends to determine the conventional true value of the BS&W from the total height of the liquid column in the auditor tank, hydrostatic pressure exerted by the liquid column, local gravity, specific mass of the water and the specific mass of the oil, and, to determine the flow, from total height of liquid column and transfer time. The calibration uses a automatized system of monitoration and data acquisition of some necessary largnesses to determine of flow and BS&W, allowing a better trustworthiness of through measurements

Fabricação de malha de trama utilizada como pré-formas na indústria de compósitos e avaliação das propriedades mecânicas

In the manufacture of composite, textile materials are being used as reinforcement. Generally, the combination of the matrix with the textile material in the form of fibres or yarns is used depending on their distribution in the web. In the present work, in place of fibres or yarns, a knitted structure in the form of the final product which is defined as preform. The preform is weft knit manufactured with polyester filaments. In the manufacture of composite, polyester resin was used as matrix. The physical and mechanical properties as well as the formability of the weft knit were analysed. The physical and mechanical properties as well as the formability of the knitted structure were analysed. The results obtained on the analysis show that the courses and wales of the weft knit structure and the tensile properties help the formability of the structure and the impregnation of the resin. It could be clearly observed that composite structure in the direction of the courses support more tension than in the direction of the wales. In relation to the three points flexural tests it was possible to note that there was more flexion in the direction of wales, what was expected. It was also possible to note that there are other advantages such as reduction in the loss of materials used, homogeneity in the distribution of the knitted structure in the mould, reduction in the preparation time and also in the reduction in the cost of manufacture

Modelagem dinâmica do escoamento de um sistema de elevação por plunger lift

A critical problem in mature gas wells is the liquid loading. As the reservoir pressure decreases, gas superficial velocities decreases and the drag exerted on the liquid phase may become insufficient to bring all the liquid to the surface. Liquid starts to drain downward, flooding the well and increasing the backpressure which decreases the gas superficial velocity and so on. A popular method to remedy this problem is the Plunger Lift. This method consists of dropping the "plunger"to the bottom of the tubing well with the main production valve closed. When the plunger reaches the well bottom the production valve is opened and the plunger carry the liquid to the surface. However, models presented in literature for predicting the behavior in plunger lift are simplistic, in many cases static (not considering the transient effects). Therefore work presents the development and validation of a numerical algorithm to solve one-dimensional compressible in gas wells using the Finite Volume Method and PRIME techniques for treating coupling of pressure and velocity fields. The code will be then used to develop a dynamic model for the plunger lift which includes the transient compressible flow within the well