148 resultados para Validation of analytical methodology


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A simple, sensitive and accurate spectrophotometric method was developed for the assay of gatifloxacin in raw material and tablets. Validation of the method yielded good results concerning range, linearity, precision and accuracy. The absorbance was measured at 287 nm for gatifloxacin tablet solutions. The linearity range was found to be 4.0-14.0 μg/mL for gatifloxacin. It was also found that the excipients in the commercial tablets did not interfere with the method.

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A simple and reproducible method was developed for the assay of lomefloxacin in tablets. The excipients in the commercial tablet preparation did not interfere with the assay. Beer's law is obeyed in the range 2.0-9.0 μg.mL-1 at λmax 280 nm. The molar absorptivity was calculated. Six triplicate analyses of solutions containing six different concentrations of the examined drug were carried out and gave a mean correlation coefficient 0.9997. The proposed method was applied to the determination of the examined drug in coated tablet and the results demonstrated that the method is equally accurate, precise and reproducible as the official methods.

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Inverted flying exercise with external loads of 25, 50, 75 and 100% of each individual maximum load in the pectoralis major and deltoideus anterior muscles was electromyographically analyzed in eleven male volunteers, using surface electrodes MEDI-TRACE-200 connected to a biological signals acquisition module coupled to a PC/AT computer. Electromyographic signals were processed and the effective values obtained were standardized through maximum voluntary isometric contraction. When the concentric phase of each muscle with the same load was statistically compared with the eccentric phase, it was observed that for all loads all the muscles presented significant electromyographic difference, and that the concentric phase was always higher. By analyzing the different loads for each muscle, it was noticed that in the concentric phase all the muscles presented significant electromyographic activity, being it higher with maximum load. When the effect of each load on different muscle in the concentric and eccentric phases was analyzed, the muscles presented a distinct activity profile.

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Within the next decade, the improved version 2 of Global Ozone Monitoring Experiment (GOME-2), a ultraviolet-visible spectrometer dedicated to the observation of key atmospheric trace species from space, will be launched successively on board three EUMETSAT Polar System (EPS) MetOp satellites. Starting with the launch of MetOp-1 scheduled for summer 2006, the GOME-2 series will extend till 2020 the global monitoring of atmospheric composition pioneered with ERS-2 GOME-1 since 1995 and enhanced with Envisat SCIAMACHY since 2002 and EOS-Aura OMI since 2004. For more than a decade, an international pool of scientific teams active in ground-and space-based ultraviolet-visible remote sensing have contributed to the successful post-launch validation of trace gas data products and the associated maturation of retrieval algorithms for the latter satellites, ensuring that geophysical data products are/become reliable and accurate enough for intended research and applications. Building on this experience, this consortium plans now to develop and carry out appropriate validation of a list of GOME-2 trace gas column data of both tropospheric and stratospheric relevance: nitrogen dioxide (NO 2), ozone (O 3), bromine monoxide (BrO), chlorine dioxide (OClO), formaldehyde (HCHO), and sulphur dioxide (SO 2). The proposed investigation will combine four complementary approaches resulting in an end-to-end validation of expected column data products.

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The electromyographic activity of the deltoideus (anterior portion) and pectoralis major (clavicular portion) muscles was analyzed in 24 male volunteers in two different modalities of pull-over exercises. The PMC activity varied from weak to moderate in both modalities, while the DA activity was moderate in the pull-over and strong in the pull-over with bent arms exercises.

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Behavioral problems in preschool children are one of the most frequent motives for seeking psychological care by parents and caregivers. Instruments are considered necessary, created from a Social Skills Training theoretical-practical perspective, which may systematically assist the identification of social skills and behavioral deficits, helping professionals in the prevention and/or reduction of behavioral problems. The purpose of this study was to test the psychometric validity and reliability of an instrument for evaluation of Socially Skilled Responses, from a teacher's perspective (QRSH-PR For this purpose, 260 preschool children were evaluated, differentiated in subgroups without and without behavioral difficulties, based on the Child Behavior Scale (Escala de Comportamento Infantil/ECI-Professor Studies were conducted for construct, discrimination, concurrent and predictive validity. The Cronbach Alpha was calculated to evaluate internal consistency. The obtained results pointed to positive indicators in reference to construct, discrimination, and predictive validity, and even for good internal consistency, indicating that the items consistently measure the construct of social skills, and differentiated children with and without behavioral problems. The questionnaire is considered to be gauged for evaluation of socially skilled responses from preschool children, and applicable in educational and clinical environments. Copyright 2009 by The Spanish Journal of Psychology.

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To carry out the dating by the Fission Track Method (FTM) the international community that works with this method employs methodologies in which the mineral to be dated must be irradiated with neutrons. Such irradiation, performed in a nuclear reactor, demand a relatively long waiting time so that the activity of the sample attain a proper level for handling. The present work aims to establish a methodology that makes possible the dating by FTM using a mass spectrometer instead of a nuclear reactor. This methodology was applied to apatite samples from Durango, Mexico. © 2009 Elsevier Ltd. All rights reserved.

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Background. From shotgun libraries used for the genomic sequencing of the phytopathogenic bacterium Xanthomonas axonopodis pv. citri (XAC), clones that were representative of the largest possible number of coding sequences (CDSs) were selected to create a DNA microarray platform on glass slides (XACarray). The creation of the XACarray allowed for the establishment of a tool that is capable of providing data for the analysis of global genome expression in this organism. Findings. The inserts from the selected clones were amplified by PCR with the universal oligonucleotide primers M13R and M13F. The obtained products were purified and fixed in duplicate on glass slides specific for use in DNA microarrays. The number of spots on the microarray totaled 6,144 and included 768 positive controls and 624 negative controls per slide. Validation of the platform was performed through hybridization of total DNA probes from XAC labeled with different fluorophores, Cy3 and Cy5. In this validation assay, 86% of all PCR products fixed on the glass slides were confirmed to present a hybridization signal greater than twice the standard deviation of the deviation of the global median signal-to-noise ration. Conclusions. Our validation of the XACArray platform using DNA-DNA hybridization revealed that it can be used to evaluate the expression of 2,365 individual CDSs from all major functional categories, which corresponds to 52.7% of the annotated CDSs of the XAC genome. As a proof of concept, we used this platform in a previously work to verify the absence of genomic regions that could not be detected by sequencing in related strains of Xanthomonas. © 2010 Moreira et al; licensee BioMed Central Ltd.

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It was analized the deltoid muscle anterior portion and the pectoralis major clavicular portion in 24 male volunteers using a two-channel electromyograph TECA TE 4, and Hewllet Packard surface electrodes, in 4 modalities of military press exercises with open grip. The results showed high inactivity for PMC in almost all the modalities while DA developed very high levels of action potentials in all the modalities assessed.

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The intension of this paper was to review and discuss some of the current quantitative analytical procedures which are used for quality control of pharmaceutical products. The selected papers were organized according to the analytical technique employed. Several techniques like ultraviolet/visible spectrophotometry, fluorimetry, titrimetry, electroanalytical techniques, chromatographic methods (thin-layer chromatography, gas chromatography and high-performance liquid chromatography), capillary electrophoresis and vibrational spectroscopies are the main techniques that have been used for the quantitative analysis of pharmaceutical compounds. In conclusion, although simple techniques such as UV/VIS spectrophotometry and TLC are still extensively employed, HPLC is the most popular instrumental technique used for the analysis of pharmaceuticals. Besides, a review of recent works in the area of pharmaceutical analysis showed a trend in the application of techniques increasingly rapid such as ultra performance liquid chromatography and the use of sensitive and specific detectors as mass spectrometers.

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As the number of simulation experiments increases, the necessity for validation and verification of these models demands special attention on the part of the simulation practitioners. By analyzing the current scientific literature, it is observed that the operational validation description presented in many papers does not agree on the importance designated to this process and about its applied techniques, subjective or objective. With the expectation of orienting professionals, researchers and students in simulation, this article aims to elaborate a practical guide through the compilation of statistical techniques in the operational validation of discrete simulation models. Finally, the guide's applicability was evaluated by using two study objects, which represent two manufacturing cells, one from the automobile industry and the other from a Brazilian tech company. For each application, the guide identified distinct steps, due to the different aspects that characterize the analyzed distributions. © 2011 Brazilian Operations Research Society.

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Numerical modeling of the interaction among waves and coastal structures is a challenge due to the many nonlinear phenomena involved, such as, wave propagation, wave transformation with water depth, interaction among incident and reflected waves, run-up / run-down and wave overtopping. Numerical models based on Lagrangian formulation, like SPH (Smoothed Particle Hydrodynamics), allow simulating complex free surface flows. The validation of these numerical models is essential, but comparing numerical results with experimental data is not an easy task. In the present paper, two SPH numerical models, SPHysics LNEC and SPH UNESP, are validated comparing the numerical results of waves interacting with a vertical breakwater, with data obtained in physical model tests made in one of the LNEC's flume. To achieve this validation, the experimental set-up is determined to be compatible with the Characteristics of the numerical models. Therefore, the flume dimensions are exactly the same for numerical and physical model and incident wave characteristics are identical, which allows determining the accuracy of the numerical models, particularly regarding two complex phenomena: wave-breaking and impact loads on the breakwater. It is shown that partial renormalization, i.e. renormalization applied only for particles near the structure, seems to be a promising compromise and an original method that allows simultaneously propagating waves, without diffusion, and modeling accurately the pressure field near the structure.

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With the objective to know the electromyographic activity normal parameters of the deltoid (anterior portion) and pectoralis major (clavicular portion) muscles in the different modalities of military press exercises with middle grip, we analyzed 24 male volunteers using a two-channel electromyograph TECA TE 4, and Hewllet Packard surface electrodes. It was observed high inactivity levels for PMC in almost all the modalities and the concentration in the active cases, mainly, in the weak potential, while DA presented very high levels of much strong action potentials in all the modalities assessed.

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The deltoid (anterior portion) and pectoralis major (clavicular portion) were evaluated in several execution ways of military press exercises with open and middle grips in order to know their behavior pattern. It was analyzed 24 male volunteers, using a 2-channel TECA TE4 electromyograph and Hewllet Packard surface electrodes. It was observed that the execution variation with open and middle grips does not present any significant difference as for the demanding level neither for the pectoralis major muscle nor the deltoid muscle.