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

Algoritmos inteligentes para auto-correção, auto-verificação e auto-validação de medidas em sensores

This work presents a set of intelligent algorithms with the purpose of correcting calibration errors in sensors and reducting the periodicity of their calibrations. Such algorithms were designed using Artificial Neural Networks due to its great capacity of learning, adaptation and function approximation. Two approaches willbe shown, the firstone uses Multilayer Perceptron Networks to approximate the many shapes of the calibration curve of a sensor which discalibrates in different time points. This approach requires the knowledge of the sensor s functioning time, but this information is not always available. To overcome this need, another approach using Recurrent Neural Networks was proposed. The Recurrent Neural Networks have a great capacity of learning the dynamics of a system to which it was trained, so they can learn the dynamics of a sensor s discalibration. Knowingthe sensor s functioning time or its discalibration dynamics, it is possible to determine how much a sensor is discalibrated and correct its measured value, providing then, a more exact measurement. The algorithms proposed in this work can be implemented in a Foundation Fieldbus industrial network environment, which has a good capacity of device programming through its function blocks, making it possible to have them applied to the measurement process

A methodology for building energy modelling and calibration in warm climates

PEDRINI, Aldomar; WESTPHAL, F. S.; LAMBERT, R.. A methodology for building energy modelling and calibration in warm climates. Building And Environment, Australia, n. 37, p.903-912, 2002. Disponível em: . Acesso em: 04 out. 2010.

Nanosistemas de penicilina G benzatina para tratamento profilático da febre reumática: estudo analítico

Investigations in the field of pharmaceutical analysis and quality control of medicines require analytical procedures with good perfomance characteristics. Calibration is one of the most important steps in chemical analysis, presenting direct relation to parameters such as linearity. This work consisted in the development of a new methodology to obtain calibration curves for drug analysis: the stationary cuvette one. It was compared to the currently used methodology, and possible sources of variation between them were evaluated. The results demonstrated that the proposed technique presented similar reproducibility compared to the traditional methodology. In addition to that, some advantages were observed, such as user-friendliness, cost-effectiveness, accuracy, precision and robustness. Therefore, the stationary cuvette methodology may be considered the best choice to obtain calibration curves for drug analyis by spectrophotometry

Bolton freeware: aplicativo de avaliação de discrepância de massa dentária desenvolvido pelo programa de pós-graduação em odontologia/UFRN

The calculation of tooth mass discrepancy, essential for good planning and a proper orthodontic finishing, when performed manually, besides being laborious, requires considerable time consumption. The aim of this study was to develop and test Bolton Freeware, a software for analysis of the tooth mass discrepancy of Bolton, aiming to minimize the consumption of time in a less onerous way. The digital analysis of the software was done by means of two-dimensional scanning of plaster study models and compared to manual evaluation (gold standard), using 75 pairs of stone plaster study models divided into two groups according to the magnitude of the Curve of Spee (group I from 0 to 2 mm, group II greater than 2 to 3mm). All the models had permanent dentition and were in perfect condition. The manual evaluation was performed with a digital caliper and a calculator, and the time required to perform the analysis for both methods was recorded and compared. In addition, the software was evaluated by orthodontists regarding its use, by means of questionnaires developed specifically for this purpose. Calibration was performed prior to manual analysis, and excellent levels of inter-rater agreement were achieved, with ICC > 0.75 and r > 0.9 for total and anterior proportion. It was observed in the evaluation of error of the digital method that some teeth showed a significant systematic error, being the highest measured at 0.08 mm. The analysis of total tooth mass discrepancy performed by Bolton Freeware, for those cases in which the curve of Spee is mild and moderate, differ from manual analysis, on average, 0.09 mm and 0.07 mm respectively, for each tooth evaluated, with r> 0, 8 for total and anterior proportion. According to the specificity and sensitivity test, Bolton Freeware has an improved ability to detect true negatives, i.e. the presence of discrepancy. The Bolton analysis digitally performed was faster, with an average difference of time consumed to perform the analysis of Bolton between the two methods of approximately 6 minutes. Most experts interviewed (93%) approved the usability of the software