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

Um estudo sobre a concepção de paradoxo segundo o pensamento de Augustus de Morgan

This work aims to analyze the concept of "paradox" posed in the work of The Budget Paradox (1872) of mathematical and logical English Augustus De Morgan (1806-1871). Here it is important to note that a large part of this book consists of re-prints of a series of writings by the author in journal Athenaeum, where its performance as auditor of literature. The tests refer to some scientific work produced between the years 1489 and 1866 and the rules of selection for the composition of the work is, basically, the methodological aspects used in the completion or disclosed by such scholars. The concept of paradox is presented in two distinct moments. At first, we found a study of definitions for the term in a philosophical approach, characterizing it as something that requires further investigation; which was complemented with the classic examples of a scientific context. In the second, we present a concept advocated by De Morgan and, under this perspective, that he conceptualized the "paradox" is directly related to the non-usual methods employed in the formulation of new scientific theories. In this study some of these scientific concepts are detailed, where, through the redemption history, engaging in issues of our study Mathematics, Physics, of Logic, among others. Possession of the preliminary analysis and comparison with the design of De Morgan, it became possible to diagnose some limitations in the conceptualization suggested by the author. Further, evidenced, in front of the cases, the nonlinearity of the process of production of knowledge and hence the progress of science

Análise não-linear de treliças pelo método dos elementos finitos posicional

This work presents the positional nonlinear geometric formulation for trusses using different strain measures. The positional formulation presents an alternative approach for nonlinear problems. This formulation considers nodal positions as variables of the nonlinear system instead of displacements (widely found in literature). The work also describes the arc-length method used for tracing equilibrium paths with snap-through and snap-back. Numerical applications for trusses already established in the literature and comparisons with other studies are provided to prove the accuracy of the proposed formulation

Uma fundamentação matemática para processamento digital de sinais intervalares

This work deals with a mathematical fundament for digital signal processing under point view of interval mathematics. Intend treat the open problem of precision and repesention of data in digital systems, with a intertval version of signals representation. Signals processing is a rich and complex area, therefore, this work makes a cutting with focus in systems linear invariant in the time. A vast literature in the area exists, but, some concepts in interval mathematics need to be redefined or to be elaborated for the construction of a solid theory of interval signal processing. We will construct a basic fundaments for signal processing in the interval version, such as basic properties linearity, stability, causality, a version to intervalar of linear systems e its properties. They will be presented interval versions of the convolution and the Z-transform. Will be made analysis of convergences of systems using interval Z-transform , a essentially interval distance, interval complex numbers , application in a interval filter.

Uma fundamentação para sinais e sistemas intervalares

In this work we use Interval Mathematics to establish interval counterparts for the main tools used in digital signal processing. More specifically, the approach developed here is oriented to signals, systems, sampling, quantization, coding and Fourier transforms. A detailed study for some interval arithmetics which handle with complex numbers is provided; they are: complex interval arithmetic (or rectangular), circular complex arithmetic, and interval arithmetic for polar sectors. This lead us to investigate some properties that are relevant for the development of a theory of interval digital signal processing. It is shown that the sets IR and R(C) endowed with any correct arithmetic is not an algebraic field, meaning that those sets do not behave like real and complex numbers. An alternative to the notion of interval complex width is also provided and the Kulisch- Miranker order is used in order to write complex numbers in the interval form enabling operations on endpoints. The use of interval signals and systems is possible thanks to the representation of complex values into floating point systems. That is, if a number x 2 R is not representable in a floating point system F then it is mapped to an interval [x;x], such that x is the largest number in F which is smaller than x and x is the smallest one in F which is greater than x. This interval representation is the starting point for definitions like interval signals and systems which take real or complex values. It provides the extension for notions like: causality, stability, time invariance, homogeneity, additivity and linearity to interval systems. The process of quantization is extended to its interval counterpart. Thereafter the interval versions for: quantization levels, quantization error and encoded signal are provided. It is shown that the interval levels of quantization represent complex quantization levels and the classical quantization error ranges over the interval quantization error. An estimation for the interval quantization error and an interval version for Z-transform (and hence Fourier transform) is provided. Finally, the results of an Matlab implementation is given

Controlador preditivo não linear aplicado ao controle de golfadas em processos de produção de petróleo

Slugging is a well-known slugging phenomenon in multiphase flow, which may cause problems such as vibration in pipeline and high liquid level in the separator. It can be classified according to the place of its occurrence. The most severe, known as slugging in the riser, occurs in the vertical pipe which feeds the platform. Also known as severe slugging, it is capable of causing severe pressure fluctuations in the flow of the process, excessive vibration, flooding in separator tanks, limited production, nonscheduled stop of production, among other negative aspects that motivated the production of this work . A feasible solution to deal with this problem would be to design an effective method for the removal or reduction of the system, a controller. According to the literature, a conventional PID controller did not produce good results due to the high degree of nonlinearity of the process, fueling the development of advanced control techniques. Among these, the model predictive controller (MPC), where the control action results from the solution of an optimization problem, it is robust, can incorporate physical and /or security constraints. The objective of this work is to apply a non-conventional non-linear model predictive control technique to severe slugging, where the amount of liquid mass in the riser is controlled by the production valve and, indirectly, the oscillation of flow and pressure is suppressed, while looking for environmental and economic benefits. The proposed strategy is based on the use of the model linear approximations and repeatedly solving of a quadratic optimization problem, providing solutions that improve at each iteration. In the event where the convergence of this algorithm is satisfied, the predicted values of the process variables are the same as to those obtained by the original nonlinear model, ensuring that the constraints are satisfied for them along the prediction horizon. A mathematical model recently published in the literature, capable of representing characteristics of severe slugging in a real oil well, is used both for simulation and for the project of the proposed controller, whose performance is compared to a linear MPC

Construção, calibração e análise de desempenho de um piranômetro de baixo custo, baseado no modelo Kimball-Hobbs

In this work a pyrometer using the classic model of Kimball-Hobbs was developed, tested and calibrated. The solar radiation is verified through the temperature difference between the sensible elements covered by absorbing (black) and reflecting (white) pigmentations of the incoming radiation. The photoacoustic technique was used to optimize the choice of the pigments. Methodologies associated with linearity, thermo-variation, sensibility, response time and distance are also presented. To correctly classify the results, the international standard ISO 9060 as well as indicative parameters of World Meteorological Organization (WMO) are used. In addition a system of data acquisition of two channels with 12 bits, constructed during the this time, was used to measure the global solar radiation on the ground by the pyrometer and also by another pyrometer certified in the case of Keep & zonen. The results statistically show, through the hypothesis test presented here, that both equipments find population average with 95% of correctness

Controle inteligente de sistemas eletroidráulicos utilizando redes neurais artificiais

This work describes the development of a nonlinear control strategy for an electro-hydraulic actuated system. The system to be controlled is represented by a third order ordinary differential equation subject to a dead-zone input. The control strategy is based on a nonlinear control scheme, combined with an artificial intelligence algorithm, namely, the method of feedback linearization and an artificial neural network. It is shown that, when such a hard nonlinearity and modeling inaccuracies are considered, the nonlinear technique alone is not enough to ensure a good performance of the controller. Therefore, a compensation strategy based on artificial neural networks, which have been notoriously used in systems that require the simulation of the process of human inference, is used. The multilayer perceptron network and the radial basis functions network as well are adopted and mathematically implemented within the control law. On this basis, the compensation ability considering both networks is compared. Furthermore, the application of new intelligent control strategies for nonlinear and uncertain mechanical systems are proposed, showing that the combination of a nonlinear control methodology and artificial neural networks improves the overall control system performance. Numerical results are presented to demonstrate the efficacy of the proposed control system

Controle por modos deslizantes com compensação difusa aplicado a sistemas com descontinuidade

The development of non-linear controllers gained space in the theoretical ambit and of practical applications on the moment that the arising of digital computers enabled the implementation of these methodologies. In comparison with the linear controllers more utilized, the non -linear controllers present the advantage of not requiring the linearity of the system to determine the parameters of control, which permits a more efficient control especially when the system presents a high level of non-linearity. Another additional advantage is the reduction of costs, since to obtain the efficient control through linear controllers it is necessary the utilization of sensors and more refined actuators than when it is utilized a non-linear controller. Among the non-linear theories of control, the method of control by gliding ways is detached for being a method that presents more robustness, before uncertainties. It is already confirmed that the adoption of compensation on the region of residual error permits to improve better the performance of these controllers. So, in this work it is described the development of a non-linear controller that looks for an association of strategy of control by gliding ways, with the fuzzy compensation technique. Through the implementation of some strategies of fuzzy compensation, it was searched the one which provided the biggest efficiency before a system with high level of nonlinearities and uncertainties. The electrohydraulic actuator was utilized as an example of research, and the results appoint to two configurations of compensation that permit a bigger reduction of the residual error

Estudo da decomposição de plantas aquáticas em função das quantidades depositadas, da umidade e do tipo de disposição no solo

Um estudo foi realizado com a finalidade de avaliar a decomposição da biomassa de plantas aquáticas, incorporadas ou não ao solo, provenientes do controle mecânico, no reservatório da UHE Americana. O ensaio foi realizado em casa de vegetação, localizada no Núcleo de Pesquisas Avançadas em Matologia (NUPAM) da FCA/Unesp-Botucatu. A avaliação foi conduzida em vasos contendo 14 kg de solo, simulando descartes de 50, 100, 150 e 200 t MF de plantas ha-1 e avaliando o processo de decomposição através da liberação de CO2, divididos em duas etapas: a primeira em solo seco e, a segunda, na seqüência, com o solo úmido. A quantificação do CO2 liberado foi realizada através de titulação de solução adicionada ao processo de incubação de 24 horas dos vasos. Os dados foram interpolados e analisados seguindo modelo de Mitscherlich, com algumas modificações. Na primeira etapa, foi observada uma rápida liberação de CO2 até o décimo dia, seguida de estabilização. O maior teor de CO2 liberado foi observado no tratamento com descarte de 200 t MF ha-1 incorporado ao solo. Os dados avaliados durante a segunda fase do ensaio representaram uma maior linearidade no processo de liberação de CO2, indicando um período mais longo do processo de degradação da biomassa descartada.

Recuperação e purificação de proteínas do soro de queijo tipo coalho usando cromatografia de troca iônica e interação hidrofóbica em leito na forma expandida

Expanded Bed Adsorption plays an important role in the downstream processing mainly for reducing costs as well as steps besides could handling cells homogenates or fermentation broth. In this work Expanded Bed Adsorption was used to recover and purify whey proteins from coalho cheese manufacture using Streamline DEAE and Streamline SP both ionic resins as well as a hydrophobic resin Streamline Phenyl. A column of 2.6 cm inner diameter with 30 cm in height was coupled to a peristaltic pump. Hydrodynamics study was carried out with the three resins using Tris-HCl buffer in concentration of 30, 50 and 70 mM, with pH ranging from 7.0 to 8.0. In this case, assays of the expansion degree as well as Residence Time Distribution (RTD) were carried out. For the recovery and purification steps, a whey sample of 200 mL, was submitted to a column with 25mL of resin previously equilibrated with Tris/HCl (50 mM, pH 7.0) using a expanded bed. After washing, elution was carried out according the technique used. For ionic adsorption elution was carried out using 100 mL of Tris/HCl (50 mM, pH 7.0 in 1M NaCl). For Hydrophobyc interaction elution was carried out using Tris/HCl (50 mM, pH 7.0). Adsorption runs were carried out using the three resins as well as theirs combination. Results showed that for hydrodynamics studies a linear fit was observed for the three resins with a correlation coefficient (R2) about 0.9. In this case, Streamline Phenyl showed highest expansion degree reaching an expansion degree (H0/H) of 2.2. Bed porosity was of 0.7 when both resins Streamline DEAE and Streamline SP were used with StremLine Phenyl showing the highest bed porosity about 0.75. The number of theorical plates were 109, 41.5 and 17.8 and the axial dipersion coefficient (Daxial) were 0.5, 1.4 and 3.7 x 10-6 m2/s, for Streamline DEAE, Streamline SP and Streamline Phenyl, respectively. Whey proteins were adsorved fastly for the three resins with equilibrium reached in 10 minutes. Breakthrough curves showed that most of proteins stays in flowthrough as well as washing steps with 84, 77 and 96%, for Streamline DEAE, Streamline SP and Streamline Phenyl, respectively. It was observed protein peaks during elution for the three resins used. According to these peaks were identified 6 protein bands that could probably be albumin (69 KDa), lactoferrin (76 KDa), lactoperoxidase (89 KDa), β-lactoglobulin (18,3 KDa) e α-lactoalbumin (14 KDa), as well as the dimer of beta-lactoglobulin. The combined system compound for the elution of Streamline DEAE applied to the Streamline SP showed the best purification of whey proteins, mainly of the α-lactoalbumina

Abordando as relações ctsa no ensino da química a partir das crenças e atitudes de licenciandos: uma experiência ormativa no Sertão Nordestino

Este estudio investigó las actitudes y creencias de los estudiantes universitarios en Ciencias Químicas por la Universidad de Río Grande do Norte (UERN) como un paso hacia la elaboración de una propuesta de material didáctico para el estudio de las relaciones CTSA en la licenciatura en química. Para el conocimiento de las actitudes y creencias fue utilizado dos instrumentos (Escala Likert y un cuestionario), que proporcionó un análisis dentro del nuevo paradigma de investigación (cuantitativa y cualitativa) en la Enseñanza de la Ciencia y Matemáticas. Los resultados mostraron que los estudiantes de licenciatura en química tienen creencias positivistas y que suelen son considerados por algunos como ingenuas, como la creencia en el modelo de decisión tecnocrática, la linealidad del desarrollo científico y tecnológico que lleva a el bienestar social y neutralidad de los conocimientos científicotecnológico. Basándose en estos datos y la literatura sobre el tema se elaboraron tres módulos de aprendizaje: a) Cuestionando la hegemonía del conocimiento técnico y científico, b) Las relaciones entre ciencia, tecnología, sociedad y medio ambiente - las relaciones CTSA c) Propuesta de temática para la enseñanza de la química en una perspectiva de CTSA: El Río Mossoró. Por último, el material producido se utilizó en dos cursos ocurridos en el Campus Central en el Centro de Educación Superior en São Miguel, ambos de UERN. Los participantes expresaron su aprobación al enfoque trajo de el experimento propuesto y de el caso de simulación contenidos en la propuesta de

Total polyphenols from Syzygium cumini (L.) Skeels fruit extract

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Development and validation of HPLC method for analysis of dexamethasone acetate in microemulsions

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Migração de ε-caprolactama de embalagens contendo poliamida 6 para simulante ácido acético 3% e validação do método analítico

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)