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

Modelo 2,5D de predição de propagação para ambientes interiores utilizando o método do traçado de raios

A 2.5D ray-tracing propagation model is proposed to predict radio loss in indoor environment. Specifically, we opted for the Shooting and Bouncing Rays (SBR) method, together with the Geometrieal Theory of Diffrartion (GTD). Besides the line-of-sight propagation (LOS), we consider that the radio waves may experience reflection, refraction, and diffraction (NLOS). In the Shooting and Bouncing Rays (SBR) method, the transmitter antenna launches a bundle of rays that may or may not reach the receiver. Considering the transmitting antenna as a point, the rays will start to launch from this position and can reach the receiver either directly or after reflections, refractions, diffractions, or even after any combination of the previous effects. To model the environment, a database is built to record geometrical characteristics and information on the constituent materials of the scenario. The database works independently of the simulation program, allowing robustness and flexibility to model other seenarios. Each propagation mechanism is treated separately. In line-of-sight propagation, the main contribution to the received signal comes from the direct ray, while reflected, refracted, and diffracted signal dominate when the line-of-sight is blocked. For this case, the transmitted signal reaches the receiver through more than one path, resulting in a multipath fading. The transmitting channel of a mobile system is simulated by moving either the transmitter or the receiver around the environment. The validity of the method is verified through simulations and measurements. The computed path losses are compared with the measured values at 1.8 GHz ftequency. The results were obtained for the main corridor and room classes adjacent to it. A reasonable agreement is observed. The numerical predictions are also compared with published data at 900 MHz and 2.44 GHz frequencies showing good convergence

Modelos matemáticos para estimativa do consumo máximo de oxigênio pela ventilometria de esforço em indivíduos saudáveis

The relation between metabolic demand and maximal oxygen consumption during exercise have been investigated in different areas of knowledge. In the health field, the determination of maximal oxygen consumption (VO2max) is considered a method to classify the level of physical fitness or the risk of cardiocirculatory diseases. The accuracy to obtain data provides a better evaluation of functional responses and allows a reduction in the error margin at the moment of risk classification, as well as, at the moment of determination of aerobic exercise work load. In Brasil, the use of respirometry associated to ergometric test became an opition in the cardiorespiratory evaluation. This equipment allows predictions concerning the oxyredutase process, making it possible to identify physiological responses to physical effort as the respiratory threshold. This thesis focused in the development of mathematical models developed by multiple regression validated by the stepwise method, aiming to predict the VO2max based on respiratory responses to physical effort. The sample was composed of a ramdom sample of 181 healthy individuals, men and women, that were randomized to two groups: regression group and cross validation group (GV). The voluntiars were submitted to a incremental treadmill test; objetiving to determinate of the second respiratory threshold (LVII) and the Peak VO2max. Using the método forward addition method 11 models of VO2max prediction in trendmill were developded. No significative differences were found between the VO2max meansured and the predicted by models when they were compared using ANOVA One-Way and the Post Hoc test of Turkey. We concluded that the developed mathematical models allow a prediction of the VO2max of healthy young individuals based on the LVII

Educação corporativa para Micro e Pequenas empresas: aplicação do MADEC em empresas do setor supermercadista

This study searches to supply an existing gap in the empirical research about the performance of controllers of Micron and Small Companies (MSCs) in the context of corporative education (EC) through the Method of Support of Decision in Corporative Education (MSDCE). In the context of MCSs, this is a pioneering work, for other works related to this thematic searched in literature are limited to conjecture the possibility of its implantation via cooperation between companies; moreover, they do not apply any type of diagnosis method or viability. The object of study is an association of supermarkets of the city of Natal/RN, composed by 16 stores, of what 14 had been searched. The main objective of this work was to apply the first stage of the MSDCE and to verify the possibility of implanting the Corporative Education in the searched MSCs. As a result, it was obtained the profile of the companies and the validation of the above-mentioned Method. The phase of diagnosis conceived through the implantation of the first stage occurred through visits to the stores, interviews, application of questionnaires and place observation. The first stage - strategical analysis for professional education - was divided in two phases: analysis of the current corporative situation and available identification of the involved difficulties and resources. The implantation of the first stage of the MSDCE in the Association of Supermarkets Parceiros da Economia demanded a mapping of abilities and demonstrated how the education management works, the main difficulties and limitations of the MCSs of the supermerket branch of Natal/RN. Beyond the technological aspects, it was verified that cultural and educational aspects need to be worked to reach efficiency in the process of implantation of a corporative education program

Desenvolvimento de um modelo computacional para a ampliação do atendimento do Programa de Acessibilidade Especial Porta a Porta - PRAE

Worldwide, the demand for transportation services for persons with disabilities, the elderly, and persons with reduced mobility have increased in recent years. The population is aging, governments need to adapt to this reality, and this fact could mean business opportunities for companies. Within this context is inserted the Programa de Acessibilidade Especial porta a porta PRAE, a door to door public transportation service from the city of Natal-RN in Brazil. The research presented in this dissertation seeks to develop a programming model which can assist the process of decision making of managers of the shuttle. To that end, it was created an algorithm based on methods of generating approximate solutions known as heuristics. The purpose of the model is to increase the number of people served by the PRAE, given the available fleet, generating optimized schedules routes. The PRAE is a problem of vehicle routing and scheduling of dial-a-ride - DARP, the most complex type among the routing problems. The validation of the method of resolution was made by comparing the results derived by the model and the currently programming method. It is expected that the model is able to increase the current capacity of the service requests of transport

Uma linguagem de modelagem da interação para auxiliar a comunicação designer-usuário

The development of interactive systems involves several professionals and the integration between them normally uses common artifacts, such as models, that drive the development process. In the model-driven development approach, the interaction model is an artifact that includes the most of the aspects related to what and how the user can do while he/she interacting with the system. Furthermore, the interactive model may be used to identify usability problems at design time. Therefore, the central problematic addressed by this thesis is twofold. In the first place, the interaction modeling, in a perspective that helps the designer to explicit to developer, who will implement the interface, the aspcts related to the interaction process. In the second place, the anticipated identification of usability problems, that aims to reduce the application final costs. To achieve these goals, this work presents (i) the ALaDIM language, that aims to help the designer on the conception, representation and validation of his interactive message models; (ii) the ALaDIM editor, which was built using the EMF (Eclipse Modeling Framework) and its standardized technologies by OMG (Object Management Group); and (iii) the ALaDIM inspection method, which allows the anticipated identification of usability problems using ALaDIM models. ALaDIM language and editor were respectively specified and implemented using the OMG standards and they can be used in MDA (Model Driven Architecture) activities. Beyond that, we evaluated both ALaDIM language and editor using a CDN (Cognitive Dimensions of Notations) analysis. Finally, this work reports an experiment that validated the ALaDIM inspection method

Geração de casos de teste a partir de especificações B

With the increasing complexity of software systems, there is also an increased concern about its faults. These faults can cause financial losses and even loss of life. Therefore, we propose in this paper the minimization of faults in software by using formally specified tests. The combination of testing and formal specifications is gaining strength in searches mainly through the MBT (Model-Based Testing). The development of software from formal specifications, when the whole process of refinement is done rigorously, ensures that what is specified in the application will be implemented. Thus, the implementation generated from these specifications would accurately depict what was specified. But not always the specification is refined to the level of implementation and code generation, and in these cases the tests generated from the specification tend to find fault. Additionally, the generation of so-called "invalid tests", ie tests that exercise the application scenarios that were not addressed in the specification, complements more significantly the formal development process. Therefore, this paper proposes a method for generating tests from B formal specifications. This method was structured in pseudo-code. The method is based on the systematization of the techniques of black box testing of boundary value analysis, equivalence partitioning, as well as the technique of orthogonal pairs. The method was applied to a B specification and B test machines that generate test cases independent of implementation language were generated. Aiming to validate the method, test cases were transformed manually in JUnit test cases and the application, created from the B specification and developed in Java, was tested. Faults were found with the execution of the JUnit test cases

Validação de um método auxiliar de diagnóstico como preditivo da presença de cárie de dentina em dentes decíduos

Esse estudo se propôs a avaliar um método auxiliar de diagnóstico (DIAGNOdent®) na predição de cárie de dentina em dentes decíduos, através de validação histológica e de microdureza. Verificando possíveis diferenças entre os valores obtidos através do método auxiliar, além de determinar um ponto de corte para parada de remoção de tecido cariado. A amostra do estudo foi de 15 crianças que apresentaram 21 cavidades de cárie, tratadas e analisadas desde antes da realização da restauração até quando da exodontia do elemento dentário. Os espécimes foram analisados através do DIAGNOdent® antes da abertura das cavidades, após a remoção do tecido cariado e depois da reabertura das cavidades que se deu após a exodontia dos elementos dentários. Posteriormente, receberam preparo metalográfico para realização de testes de microdureza e microscopia óptica que serviram como forma de validação para as mensurações obtidas pela fluorescência a laser. Houve diferença significativa entre os valores DIAGNOdent® encontrados antes da abertura da cavidade e os demais (p < 0,0001). Havendo correlação significativa (r = 0,432 ; p = 0,019) apenas para as aferições obtidas antes da abertura das cavidades e quando do término da remoção do tecido cariado. Para a microdureza, as médias axiais foram significativamente maiores que as pulpares, existindo correlação entre a microdureza pulpar e os valores do DIAGNOdent® após a reabertura (r = - 0,472 ; p = 0,002). Valores de 15,38% para a sensibilidade, 100% para a especificidade, 100% para o valor preditivo positivo e 71,79% para o valor preditivo negativo, foram obtidos quando se utilizou um ponto de corte de 30 para fluorescência a laser, tendo como padrão-ouro a microdureza pulpar. Partindo da média dos valores de fluorescência a laser obtidos após a remoção do tecido cariado e acrescentando-se um desvio-padrão a esta, o método indicou o valor de 19 como ponto de corte para cessar a remoção de dentina. Concluiu-se que, nas condições analisadas, o método auxiliar de diagnóstico (DIAGNOdent®) é um método acurado na predição de cárie de dentina em dentes decíduos. Além disso, o método comprovou que o padrão usual de remoção de dentina garante a remoção do tecido cariado

Satisfação do paciente com a fisioterapia :tradução, adequação cultura e validação de um instrumento de medida

The measurement of patient satisfaction can provide information about the success of the care provider in reaching the values and meeting the expectations of the patient. The purpose of this study was to translate into the Portuguese language and to culturally customize to the Brazilian population the instrument to measure patient satisfaction with physical therapy elaborated by Goldstein et al. The study sample was made up of 279 patients who were undergoing physical therapy treatment at 39 different private clinics in a middle-sized town in northeastern Brazil. For the translation of the survey instrument, the back-translation technique was employed, in association with the bilingual method. The reliability and validity of the Brazilian version of the instrument were both assessed. Reliability analysis, carried out with the computation of Cronbach alpha coefficients, showed that the measures obtained with the instrument have a high degree of internal consistency. The aspects dealing with the patient therapist relationship are the most important predictors of satisfaction, followed by those dealing with courtesy, privacy, and practical aspects such as efficiency of the facility in the patient admissions process, setting up of appointments, and waiting time in waiting room. Items dealing with aspects such as location of the facility and availability of parking facilities may underestimate the reliability of the instrument. This study translated, culturally customized, and validated an instrument to measure patient satisfaction with physical therapy originally developed in English. By so doing, this study has made this instrument available to the Brazilian society, and it has rendered it a useful parameter that can be utilized in our country in the field of physical therapy

Avaliação de um método de cromatografia em fase gasosa head space e estudo da estabilidade do etanol em amostras de sangue

The ethanol is the most overused psychoactive drug over the world; this fact makes it one of the main substances required in toxicological exams nowadays. The development of an analytical method, adaptation or implementation of a method known, involves a process of validation that estimates its efficiency in the laboratory routine and credibility of the method. The stability is defined as the ability of the sample of material to keep the initial value of a quantitative measure for a defined period within specific limits when stored under defined conditions. This study aimed to evaluate the method of Gas chromatography and study the stability of ethanol in blood samples, considering the variables time and temperature of storage, and the presence of preservative and, with that check if the conditions of conservation and storage used in this study maintain the quality of the sample and preserve the originally amount of analyte present. Blood samples were collected from 10 volunteers to evaluate the method and to study the stability of ethanol. For the evaluation of the method, part of the samples was added to known concentrations of ethanol. In the study of stability, the other side of the pool of blood was placed in two containers: one containing the preservative sodium fluoride 1% and the anticoagulant heparin and the other only heparin, was added ethanol at a concentration of 0.6 g/L, fractionated in two bottles, one being stored at 4ºC (refrigerator) and another at -20ºC (freezer), the tests were performed on the same day (time zero) and after 1, 3, 7, 14, 30 and 60 days of storage. The assessment found the difference in results during storage in relation to time zero. It used the technique of headspace associated with gas chromatography with the FID and capillary column with stationary phase of polyethylene. The best analysis of chromatographic conditions were: temperature of 50ºC (column), 150ºC (jet) and 250ºC (detector), with retention time for ethanol from 9.107 ± 0.026 and the tercbutanol (internal standard) of 8.170 ± 0.081 minutes, the ethanol being separated properly from acetaldehyde, acetone, methanol and 2-propanol, which are potential interfering in the determination of ethanol. The technique showed linearity in the concentration range of 0.01 and 3.2 g/L (0.8051 x + y = 0.6196; r2 = 0.999). The calibration curve showed the following equation of the line: y = x 0.7542 + 0.6545, with a linear correlation coefficient equal to 0.996. The average recovery was 100.2%, the coefficients of variation of accuracy and inter intra test showed values of up to 7.3%, the limit of detection and quantification was 0.01 g/L and showed coefficient of variation within the allowed. The analytical method evaluated in this study proved to be fast, efficient and practical, given the objective of this work satisfactorily. The study of stability has less than 20% difference in the response obtained under the conditions of storage and stipulated period, compared with the response obtained at time zero and at the significance level of 5%, no statistical difference in the concentration of ethanol was observed between analysis. The results reinforce the reliability of the method of gas chromatography and blood samples in search of ethanol, either in the toxicological, forensic, social or clinic

Uma aplicação de análise de decisão com o método AHP Processo de hierarquia analítica: um estudo sobre adoção de Sistema eletrônico de cobrança no Transporte público urbano

This thesis carries through an application of Analysis of Multicriterion Decision with use of the method of Analytical Hierarchy Process (AHP) in the problematic one of taking of decision of the adoption of electronic collecting in the system of urban transport in the country, a subject that has been controversial. A modeling of criteria and alternatives is carried through and applied a questionnaire based on method AHP the excellent actors in the system of urban transport - Leading of the Managing Agency Public Municipal theatre of Urban Transports, Controller of Company of Bus, Controller of Labor union, Controller of Union of Companies, Communitarian Leader. The considered alternatives were: the maintenance of the current state with collectors, the implementation of electronic collection without collectors, and the implementation of electronic collection with collectors. The used criteria were: job, impact in the fare, control of the system, easiness of use, information. The study was carried through in the city of Natal, RN, where if the adoption of electronic collection argues and where this implementation in some bus lines between Natal and Parnamirim exists, city that integrates the region of the great Natal. The main results of the method evidence in a dimension, the viability of use of method AHP with questionnaire by means of validation of the judgments with analysis of variance beyond proper the normal mechanisms of analysis of consistency to the method, and in another one, the contribution of the analysis boarding multicriterion to become the judgments more clearly. The main results of the analysis help to show that although to models of criteria and distinct judgments of the actors, the method evidenced that it has inclination the adoption of the electronic collection on the current situation, even so with divergences between the maintenance or not of the collector. The research points to the possibility of accomplishment of the application of the AHP in successive rounds of judgments

Um algoritmo para estimação de estado em alimentadores de distribuição de energia elétrica com base no método da soma de potências

Most algorithms for state estimation based on the classical model are just adequate for use in transmission networks. Few algorithms were developed specifically for distribution systems, probably because of the little amount of data available in real time. Most overhead feeders possess just current and voltage measurements at the middle voltage bus-bar at the substation. In this way, classical algorithms are of difficult implementation, even considering off-line acquired data as pseudo-measurements. However, the necessity of automating the operation of distribution networks, mainly in regard to the selectivity of protection systems, as well to implement possibilities of load transfer maneuvers, is changing the network planning policy. In this way, some equipments incorporating telemetry and command modules have been installed in order to improve operational features, and so increasing the amount of measurement data available in real-time in the System Operation Center (SOC). This encourages the development of a state estimator model, involving real-time information and pseudo-measurements of loads, that are built from typical power factors and utilization factors (demand factors) of distribution transformers. This work reports about the development of a new state estimation method, specific for radial distribution systems. The main algorithm of the method is based on the power summation load flow. The estimation is carried out piecewise, section by section of the feeder, going from the substation to the terminal nodes. For each section, a measurement model is built, resulting in a nonlinear overdetermined equations set, whose solution is achieved by the Gaussian normal equation. The estimated variables of a section are used as pseudo-measurements for the next section. In general, a measurement set for a generic section consists of pseudo-measurements of power flows and nodal voltages obtained from the previous section or measurements in real-time, if they exist -, besides pseudomeasurements of injected powers for the power summations, whose functions are the load flow equations, assuming that the network can be represented by its single-phase equivalent. The great advantage of the algorithm is its simplicity and low computational effort. Moreover, the algorithm is very efficient, in regard to the accuracy of the estimated values. Besides the power summation state estimator, this work shows how other algorithms could be adapted to provide state estimation of middle voltage substations and networks, namely Schweppes method and an algorithm based on current proportionality, that is usually adopted for network planning tasks. Both estimators were implemented not only as alternatives for the proposed method, but also looking for getting results that give support for its validation. Once in most cases no power measurement is performed at beginning of the feeder and this is required for implementing the power summation estimations method, a new algorithm for estimating the network variables at the middle voltage bus-bar was also developed

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

Construção e evidências de validação de instrumentos de pesquisa para avaliação da assistência nos centros de atenção psicossocial

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES