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

Tradução, adaptação e validação da versão brasileira do questionário utian quality of life (uqol) para avaliação da qualidade de vida no climatério

The present study had as objective translates, to do equivalence and validation of the Utian Quality of Life (UQOL) for the Brazilian population through methods internationally accepted, in which the original questionnaire was translated for the Portuguese by three teachers and the consensual version was translated back for English by two American teachers (back translation). A multidisciplinary committee evaluated all versions and the final version in Portuguese was applied to climacteric women for the process of adaptation. Validation of the instrument was performed by measuring the reliability and validity properties. Construct validity was examined through the comparison between UQOL and the general measuring scale of quality of life Short Form-36 (SF-36). The final version of translation process was easily recognized by the target population, that didn't tell understanding problems. The results obtained for the reliability intra and interobserver showed significant agreement in all of the subjects. The construct validity was obtained through correlations statistically significant among the domains occupational, health and emotional of UQOL with the SF-36 domains. For the exploratory factorial analysis, it was verified that three factors explain 60% of the total variance of the data, the present study allowed concluding that UQOL was appropriately translated and adapted for applicability in Brazil, presenting high reliability and validity. In that way, the executed project provided the involvement of different areas as gynecology, psychology and physiotherapy (interdisciplinary). Thus, this instrument can be included and used in Brazilian studies to assessment the quality of life during the climacteric years

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

Desenvolvimento e validação de protótipo das medidas de desenvolvimento humano

To mesure the human performance is a challenge, mainly due to the multidimensional factor movement. Instruments, mostly only assess one dimension of it. Objective: To develop a prototype capable of measuring the skills of human performance and check its validity using method comparison approach. Methods: The study was divided into two stages. The first Prototype was developed and tested simultaneously with an instrument to study the Rectilinear Uniform Motion and Uniformly Miscellaneous. In the second phase the sample consisted of Paralympic basketball athletes (n=09) and karate athletes (n=31) and all agreed to the terms of participation in the research. The evaluation of performance measures was performed with the prototype, the results obtained were compared with the data calculated by a statistical package is used as a reference. Results: All variables calculated by the prototype showed no significant differences when compared with the results calculated by the reference instrument and statistical package. Conclusion: The prototype has been developed and the results obtained in laboratory and field indicate that the prototype can be used for measuring human performance measures, with immediate results without the need for a conventional computer return, provided they fulfill the criteria described

Metodologia para modelagem, validação e programação de controladores lógicos industriais usando statecharts básicos

Due of industrial informatics several attempts have been done to develop notations and semantics, which are used for classifying and describing different kind of system behavior, particularly in the modeling phase. Such attempts provide the infrastructure to resolve some real problems of engineering and construct practical systems that aim at, mainly, to increase the productivity, quality, and security of the process. Despite the many studies that have attempted to develop friendly methods for industrial controller programming, they are still programmed by conventional trial-and-error methods and, in practice, there is little written documentation on these systems. The ideal solution would be to use a computational environment that allows industrial engineers to implement the system using high-level language and that follows international standards. Accordingly, this work proposes a methodology for plant and control modelling of the discrete event systems that include sequential, parallel and timed operations, using a formalism based on Statecharts, denominated Basic Statechart (BSC). The methodology also permits automatic procedures to validate and implement these systems. To validate our methodology, we presented two case studies with typical examples of the manufacturing sector. The first example shows a sequential control for a tagged machine, which is used to illustrated dependences between the devices of the plant. In the second example, we discuss more than one strategy for controlling a manufacturing cell. The model with no control has 72 states (distinct configurations) and, the model with sequential control generated 20 different states, but they only act in 8 distinct configurations. The model with parallel control generated 210 different states, but these 210 configurations act only in 26 distinct configurations, therefore, one strategy control less restrictive than previous. Lastly, we presented one example for highlight the modular characteristic of our methodology, which it is very important to maintenance of applications. In this example, the sensors for identifying pieces in the plant were removed. So, changes in the control model are needed to transmit the information of the input buffer sensor to the others positions of the cell

Validação de uma metodologia de ensaio de resistência ao cisalhamento para avaliação da aderência de interfaces revestimento metálico-bainha de cimento aplicada a poços de petróleo

Improving the adherence between oilwell metallic casing and cement sheath potentially decrease the number of corrective actions present/y necessary for Northeastern wells submitted to steam injection. In addition to the direct costs involved in the corrective operations, the economic impact of the failure of the primary cementing aIso includes the loss in the production of the well. The adherence between casing and cement is current/y evaluated by a simple shear tests non standardized by the American Petroleum Institute (API). Therefore, the objective of the present is to propose and evaluate a standardized method to assess the adherence of oilwell metallic casing to cement sheath. To that end, a section of a cemented oilwell was simulated and used to test the effect of different parameters on the shear stress of the system. Surface roughness and different cement compositions submitted or not to thermal cycling were evaluated. The results revealed that the test geometry and parameters proposed yielded different values for the shear stress of the system, corresponding to different adherent conditions between metallic casing and cement sheath

Validação do questionário Internacional de Atividade Física (IPAQ) através da acelerometria em idosas

Physical activity is one of the main components of a healthy lifestyle, responsible for many health benefits. Despite being considered important for both disease prevention and health promotion there is high prevalence of sedentary behavior in the elderly population. Questionnaires are practical and feasible instruments for assessing levels of physical activity. However, they may have limitations in older age ranges. Accelerometers, movement sensors that make physical activity data more objective, emerge as reliable measuring devices. Aim: Determine the validity of the International Physical Activity Questionnaire (IPAQ) adapted for elderly with accelerometry in elderly women. Methods: 57 elderly women, with mean age of 66.05 ± 5.98 years who took part in hypertension control and physical activity incentive programs were assessed in relation to objective and subjective measures of physical activity. The accelerometer was used for 07 consecutive days, 24 hours per day before the IPAQ was applied. Data were analyzed using measures of central tendency and dispersion to characterize the sample according to variables collected. To check the validity of the data we used the Spearman correlation test, considering a significance level of p <0.05. Results: With respect to the categories of physical activity obtained by IPAQ, 46.4% developed moderate physical activity, followed by a high (30.3%) and low level (23.2%). There was a negative correlation only between self-reported time spent sitting and time spent on light activities as measured by accelerometry (r = - 0.408; p = 0.003) and mean activity level (counts/min) with physical activity levels evaluated by IPAQ (r = 0.297; p = 0.036). Conclusion: The IPAQ used in elderly women shows moderate to low validity levels according to accelerometry measures. Assessment of sedentary activities exhibited acceptable levels compared to accelerometry; however, moderate (r = 0.096; p > 0.05) to vigorous (r = 0.098; p > 0.05) activities were not correlated, demonstrating the inability of IPAQ to evaluate this type of activity in elderly women

Validação da escala de fatigabilidade percebida para avaliação da fadiga em idosas

The term fatigability concerns the degree of fatigue associated with performing an activity of any type (physical, mental, emotional and / or social). Recently scales for assessing fatigue in the English language were created, however, gaps exist regarding the validity of these scales in relation to oxygen consumption and levels of perceived fatigue. Objective: To investigate the validity of perceived fatigability scale in older women frail and non-frail by the expired gases kinetics. Methods: This is a study of type validation, where were evaluated 48 elderly. The evaluation was conducted at two different sessions. In the first, data were collected demographic partners, as well as assessment of cognitive function, physical health, and the phenotype of frailty. The second was composed by the test 6-minute walk (6MWT) associated the expired gases kinects and assessment of perceived fatigability. Statistical analysis was performed a descriptive analysis and then we used the Pearson correlation test to evaluate the relationship between the measure of perceived fatigue and variables oxygen consumption (VO2), carbon dioxide production (VCO2), respiratory exchange ratio (RER)before and after 6MWT. We used a linear regression model initially considering the following explanatory variable: age, Body Mass Index (BMI), presence of frailty, comorbidities, level of physical activity, distance covered in the 6MWT , the energy cost of walking and severity of fatigability on performance. Results: The final sample consisted of 44 elderly women, 4 elderly were excluded because they didn t complete all phases of this study. The mean age obtained was 75 years (± 7.2 years). There was no significant correlation between fatigability measures and the values of VO2 ( r = .09 , p = .56 ) , VCO2 ( r = .173 , p = .26 ) , RER ( r = - .121 , p = .43 ). The final linear regression model showed that the energy cost of walking, the usual level of physical activity and the performance severity of fatigability explained 83.5 % (R2 = 0.835, p < 0.01) of the variation in the perceived fatigability. Conclusion: Our findings indicate a relationship between greater severity of fatigability and lower levels of physical activity and increased energy cost in walking, suggesting that the fatigability analyses using a simple numeric scale is valid and viable for assessment of fatigue in older women

Detecção de metamidofós em solos por métodos ecotoxicológico e cromatografia líquida acoplada à espectrometria de massas sequencial (LC-MS/MS)

Soil contamination by pesticides is an environmental problem that needs to be monitored and avoided. However, the lack of fast, accurate and low cost analytical methods for discovering residual pesticide in complex matrices, such as soil, is a problem still unresolved. This problem needs to be solved before we are able to assess the quality of environmental samples. The intensive use of pesticides has increased since the 60s, because the dependence of their use, causing biological imbalances and promoting resistance and recurrence of high populations of pests and pathogens (upwelling). This has contributed to the appearance of new pests that were previously under natural control. To develop analytical methods that are able to quantify residues pesticide in complex environment. It is still a challenge for many laboratories. The integration of two analytical methods one ecotoxicological and another chemical demonstrates the potential for environmental analysis of methamidophos. The aim of this study was to evaluate an ecotoxicological method as "screening" analytical methamidophos in the soil and perform analytical confirmation in the samples of the concentration of the analyte by chemical method LC-MS/MS In this work we tested two soils: a clayey and sandy, both in contact with the kinetic methamidophos model followed pseudo-second order. The clay soil showed higher absorption of methamidophos and followed the Freundlich model, while the sandy, the Langmuir model. The chemical method was validated LC-MS/MS satisfactory, showing all parameters of linearity, range, precision, accuracy, and sensitivity adequate. In chronic ecotoxicological tests with C. dubia, the NOEC was 4.93 and 3.24 for ng L-1 of methamidophos to elutriate assays of sandy and clay soils, respectively. The method for ecotoxicological levels was more sensitive than LC-MS/MS detection of methamidophos, loamy and sandy soils. However, decreasing the concentration of the standard for analytical methamidophos and adjusting for the validation conditions chemical acquires a limit of quantification (LOQ) in ng L-1, consistent with the provisions of ecotoxicological test. The methods described should be used as an analytical tool for methamidophos in soil, and the ecotoxicological analysis can be used as a "screening" and LC-MS/MS as confirmatory analysis of the analyte molecule, confirming the objectives of this work

Novos métodos determinísticos para gerar centros iniciais dos grupos no algoritmo fuzzy C-Means e variantes

Data clustering is applied to various fields such as data mining, image processing and pattern recognition technique. Clustering algorithms splits a data set into clusters such that elements within the same cluster have a high degree of similarity, while elements belonging to different clusters have a high degree of dissimilarity. The Fuzzy C-Means Algorithm (FCM) is a fuzzy clustering algorithm most used and discussed in the literature. The performance of the FCM is strongly affected by the selection of the initial centers of the clusters. Therefore, the choice of a good set of initial cluster centers is very important for the performance of the algorithm. However, in FCM, the choice of initial centers is made randomly, making it difficult to find a good set. This paper proposes three new methods to obtain initial cluster centers, deterministically, the FCM algorithm, and can also be used in variants of the FCM. In this work these initialization methods were applied in variant ckMeans.With the proposed methods, we intend to obtain a set of initial centers which are close to the real cluster centers. With these new approaches startup if you want to reduce the number of iterations to converge these algorithms and processing time without affecting the quality of the cluster or even improve the quality in some cases. Accordingly, cluster validation indices were used to measure the quality of the clusters obtained by the modified FCM and ckMeans algorithms with the proposed initialization methods when applied to various data sets

Algoritmos de agrupamentos fuzzy intervalares e índice de validação para agrupamento de dados simbólicos do tipo intervalo

Symbolic Data Analysis (SDA) main aims to provide tools for reducing large databases to extract knowledge and provide techniques to describe the unit of such data in complex units, as such, interval or histogram. The objective of this work is to extend classical clustering methods for symbolic interval data based on interval-based distance. The main advantage of using an interval-based distance for interval-based data lies on the fact that it preserves the underlying imprecision on intervals which is usually lost when real-valued distances are applied. This work includes an approach allow existing indices to be adapted to interval context. The proposed methods with interval-based distances are compared with distances punctual existing literature through experiments with simulated data and real data interval

Validação de espécies de Centropomus (Centropomidae, Perciformes) do litoral do Rio Grande do Norte através de caracterização citogenética e molecular

The Centropomidae family consists of three genera, Centropomus, Lates and Psammoperca. Centropomus is the most diverse group, with six Centropomus species occur in the Western Atlantic Ocean C. poeyi Chávez, 1961, C. parallelus Poey, 1860, C. mexicanus Bocourt, 1868, C. pectinatus Poey, 1860 and C. ensiferus Poey, 1860. Some of these species are considered cryptic, because of its morphological traits showed low resolution for identification purposes. Despite showing great interest as a natural resource and fish culture, aspects of their diversity and karyotypic patterns are poorly understood. In this work morphological identification and comparison of mitochondrial 16S gene sequence were used to identify the species of the genus Centropomus occurring in Rio Grande do Norte, northeastern Brazil. Two sepecies were identified, C. undecimalis and C. mexicanus, which had the chromosomal aspects analyzed, through Classical cytogenetic method analyzes (conventional staining, C-banding, Ag-NORs), fluorochrome staining AT- and GC-specific, replication bands by incorporating of the base analog 5-Bromo-2’-deoxyuridine (5-BrdU), in situ chromosomal mapping of (TTAGGG)n sequences and in situ chromosome mapping 18S and 5S rRNA genes. Both species show 2n=48 acrocentric chromosomes, with ribosomal sites (Ag-NOR/18S rDNA/ Mitramycin+) in second chromosomal pair, in telomeric position on the long arm in C. mexicanus and interstitial in C. undecimalis. The nuclear organization pair (pair 2) shown a resolutive cytotaxonomic marker for these two species. The generated data reveal a lower species diversity than previously believed, suggesting that greater attention should be paid in taxonomic identification of the species, in view of optimize commercial actions exploitation, biological conservation and cultivation.

Um estudo sobre a variabilidade do vento no nordeste do Brasil através de métodos estatísticos e via modelos dinâmicos de meso e micro escala

The objective of this study was to determine the seasonal and interannual variability and calculate the trends of wind speed in NEB and then validate the mesoscale numerical model for after engage with the microscale numerical model in order to get the wind resource at some locations in the NEB. For this we use two data sets of wind speed (weather stations and anemometric towers) and two dynamic models; one of mesoscale and another of microscale. We use statistical tools to evaluate and validate the data obtained. The simulations of the dynamic mesoscale model were made using data assimilation methods (Newtonian Relaxation and Kalman filter). The main results show: (i) Five homogeneous groups of wind speed in the NEB with higher values in winter and spring and with lower in summer and fall; (ii) The interannual variability of the wind speed in some groups stood out with higher values; (iii) The large-scale circulation modified by the El Niño and La Niña intensified wind speed for the groups with higher values; (iv) The trend analysis showed more significant negative values for G3, G4 and G5 in all seasons and in the annual average; (v) The performance of dynamic mesoscale model showed smaller errors in the locations Paracuru and São João and major errors were observed in Triunfo; (vi) Application of the Kalman filter significantly reduce the systematic errors shown in the simulations of the dynamic mesoscale model; (vii) The wind resource indicate that Paracuru and Triunfo are favorable areas for the generation of energy, and the coupling technique after validation showed better results for Paracuru. We conclude that the objective was achieved, making it possible to identify trends in homogeneous groups of wind behavior, and to evaluate the quality of both simulations with the dynamic model of mesoscale and microscale to answer questions as necessary before planning research projects in Wind-Energy area in the NEB

Desenvolvimento e validação de testes de fluxo lateral para a detecção de cultivares geneticamente modificados e de aflatoxinas em produtos agrícolas

The expansion of cultivated areas with genetically modified crops (GM) is a worldwide phenomenon, stimulating regulatory authorities to implement strict procedures to monitor and verify the presence of GM varieties in agricultural crops. With the constant growing of plant cultivating areas all over the world, consumption of aflatoxin-contaminated food also increased. Aflatoxins correspond to a class of highly toxic contaminants found in agricultural products that can have harmful effects on human and animal health. Therefore, the safety and quality evaluation of agricultural products are important issues for consumers. Lateral flow tests (strip tests) is a promising method for the detection both proteins expressed in GM crops and aflatoxins-contaminated food samples. The advantages of this technique include its simplicity, rapidity and cost-effective when compared to the conventional methods. In this study, two novel and sensitive strip tests assay were developed for the identification of: (i) Cry1Ac and Cry8Ka5 proteins expressed in GM cotton crops and; (ii) aflatoxins from agricultural products. The first strip test was developed using a sandwhich format, while the second one was developed using a competitive format. Gold colloidal nanoparticles were used as detector reagent when coated with monoclonal antibodies. An anti-species specific antibody was sprayed at the nitrocellulose membrane to be used as a control line. To validate the first strip test, GM (Bollgard I® e Planta 50- EMBRAPA) and non-GM cotton leaf (Cooker 312) were used. The results showed that the strip containing antibodies for the identification of Cry1Ac and Cry8Ka5 proteins was capable of correctly distinguishing between GM samples (positive result) and non-GM samples (negative result), in a high sensitivity manner. To validate the second strip test, artificially contaminated soybean with Aspergillus flavus (aflatoxin-producing fungus) was employed. Food samples, such as milk and soybean, were also evaluated for the presence of aflatoxins. The strip test was capable to distinguish between samples with and without aflatoxins samples, at a sensitivity concentration of 0,5 μg/Kg. Therefore, these results suggest that the strip tests developed in this study can be a potential tool as a rapid and cost-effective method for detection of insect resistant GM crops expressing Cry1Ac and Cry8Ka5 and aflatoxins from food samples.

Desenvolvimento e validação de testes de fluxo lateral para a detecção de cultivares geneticamente modificados e de aflatoxinas em produtos agrícolas

The expansion of cultivated areas with genetically modified crops (GM) is a worldwide phenomenon, stimulating regulatory authorities to implement strict procedures to monitor and verify the presence of GM varieties in agricultural crops. With the constant growing of plant cultivating areas all over the world, consumption of aflatoxin-contaminated food also increased. Aflatoxins correspond to a class of highly toxic contaminants found in agricultural products that can have harmful effects on human and animal health. Therefore, the safety and quality evaluation of agricultural products are important issues for consumers. Lateral flow tests (strip tests) is a promising method for the detection both proteins expressed in GM crops and aflatoxins-contaminated food samples. The advantages of this technique include its simplicity, rapidity and cost-effective when compared to the conventional methods. In this study, two novel and sensitive strip tests assay were developed for the identification of: (i) Cry1Ac and Cry8Ka5 proteins expressed in GM cotton crops and; (ii) aflatoxins from agricultural products. The first strip test was developed using a sandwhich format, while the second one was developed using a competitive format. Gold colloidal nanoparticles were used as detector reagent when coated with monoclonal antibodies. An anti-species specific antibody was sprayed at the nitrocellulose membrane to be used as a control line. To validate the first strip test, GM (Bollgard I® e Planta 50- EMBRAPA) and non-GM cotton leaf (Cooker 312) were used. The results showed that the strip containing antibodies for the identification of Cry1Ac and Cry8Ka5 proteins was capable of correctly distinguishing between GM samples (positive result) and non-GM samples (negative result), in a high sensitivity manner. To validate the second strip test, artificially contaminated soybean with Aspergillus flavus (aflatoxin-producing fungus) was employed. Food samples, such as milk and soybean, were also evaluated for the presence of aflatoxins. The strip test was capable to distinguish between samples with and without aflatoxins samples, at a sensitivity concentration of 0,5 μg/Kg. Therefore, these results suggest that the strip tests developed in this study can be a potential tool as a rapid and cost-effective method for detection of insect resistant GM crops expressing Cry1Ac and Cry8Ka5 and aflatoxins from food samples.