893 resultados para Rapid assessment method
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A calibration method was developed using flow injection analysis (FI) with a Gradient Calibration Method (GCM). The method allows the rapid determination of zinc In foods (approximately 30 min) after treatment with concentrated sulphuric acid and 30% hydrogen peroxide, and analysis with flame atomic absorption spectrometry (FAAS). The method provides analytical results with a relative standard deviation of about 2% and requires less time than by conventional FI calibration. The electronic selection of different segments along the gradient and monitoring of the technique covers wide concentration ranges while maintaining the inherent high precision of flow injection analysis. Concentrations, flow rates, and flow times of the reagents were optimized in order to obtain best accuracy and precision. Flow rates of 10 mL/min were selected for zinc. In addition, the system enables electronic dilution and calibration where a multipoint curve can be constructed using a single sample injection.
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This paper describes a simple, portable and environmentally friendly method for the rapid determination of dipyrone in pharmaceuticals by using diffuse reflectance spectroscopy. The proposed method is based on the reflectance measurements of the orange compound produced from the spot test reaction between dipyrone and p-dimethylaminocinnamaldehyde (p-DAC), in acid medium, using a filter paper as solid support. Experimental design methodologies were used to optimize the measurement conditions. All reflectance measurements were carried out at 510 nm and the linear range was from 1.42 × 10-4-2.85 × 10-3 mol L-1, with a correlation coefficient of 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 1.20 × 10-5 mol L-1 and 4.00 × 10-5 mol L-1, respectively. The intraday precision and interday precision were studied for 10 replicate analyses of 7.90 × 10-4 mol L-1 dipyrone solution. The coefficients of variation were 1.1 and 0.9%, respectively. The proposed method was applied successfully to the determination of dipyrone in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95% confidence level. ©2007 Sociedade Brasileira de Química.
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Includes bibliography
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This paper describes a simple, environmentally friendly and rapid quantitative spot test procedure for the determination of captopril (CPT) in bulk drug and in pharmaceutical formulations by using diffuse reflectance spectroscopy. The proposed method is based on the reflectance measurements of the orange compound (λ max 490 nm) produced by the spot test reaction between CPT and p-chloranil (CL). Under optimal conditions, calibration curves were obtained for CPT by plotting the optical density of the reflectance signal (A R) vs. the log of the mol L -1 concentration, from 6.91×10 -3 to 1.17×10 -1, with a good coefficient of determination (R 2 = 0.9992). The common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method was applied to determine CPT in commercial pharmaceutical formulations. The results obtained by the proposed method are compared favorably with those obtained by an official procedure at 95% confidence level. The method validation results showed that the sensitivity and selectivity of the methods were adequated for drug monitoring in industrial quality control laboratories. © 2011 Moment Publication.
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A numerical study of mass conservation of MAC-type methods is presented, for viscoelastic free-surface flows. We use an implicit formulation which allows for greater time steps, and therefore time marching schemes for advecting the free surface marker particles have to be accurate in order to preserve the good mass conservation properties of this methodology. We then present an improvement by using a Runge-Kutta scheme coupled with a local linear extrapolation on the free surface. A thorough study of the viscoelastic impacting drop problem, for both Oldroyd-B and XPP fluid models, is presented, investigating the influence of timestep, grid spacing and other model parameters to the overall mass conservation of the method. Furthermore, an unsteady fountain flow is also simulated to illustrate the low mass conservation error obtained.
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The objective of this study was to demonstrate the effectiveness of rugoscopy as a human identification method, even when the patient is submitted to rapid palatal expansion, which in theory would introduce doubt. With this intent, the Rugoscopic Identity was obtained for each subject using the classification formula proposed by Santos based on the intra-oral casts made before and after treatment from patients who were subjected to palatal expansion. The casts were labeled with the patients' initials and randomly arranged for studying. The palatine rugae kept the same patterns in every case studied. The technical error of the intra-evaluator measurement provided a confidence interval of 95%, making rugoscopy a reliable identification method for patients who were submitted to rapid palatal expansion, because even in the presence of intra-oral changes owing to the use of palatal expanders, the palatine rugae retained the biological and technical requirements for the human identification process. © 2012 American Academy of Forensic Sciences.
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The invasive fire ant Solenopsis invicta is medically important because its venom is highly potent. However, almost nothing is known about fire ant venom proteins because obtaining even milligram-amounts of these proteins has been prohibitively challenging. We present a simple and fast method of obtaining whole venom compounds from large quantities of fire ants. For this, we separate the ants are from the nest soil, immerse them in dual-phase mixture of apolar organic solvent and water, and evaporate each solvent phase in separate. The remaining extract from the aqueous phase is largely made up of ant venom proteins. We confirmed this by using 2D gel electrophoresis while also demonstrating that our new approach yields the same proteins obtained by other authors using less efficient traditional methods. © 2013 Elsevier Ltd.
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This paper provides a contribution to the contingency analysis of electric power systems under steady state conditions. An alternative methodology is presented for static contingency analyses that only use continuation methods and thus provides an accurate determination of the loading margin. Rather than starting from the base case operating point, the proposed continuation power flow obtains the post-contingency loading margins starting from the maximum loading and using a bus voltage magnitude as a parameter. The branch selected for the contingency evaluation is parameterised using a scaling factor, which allows its gradual removal and assures the continuation power flow convergence for the cases where the method would diverge for the complete transmission line or transformer removal. The applicability and effectiveness of the proposed methodology have been investigated on IEEE test systems (14, 57 and 118 buses) and compared with the continuation power flow, which obtains the post-contingency loading margin starting from the base case solution. In general, for most of the analysed contingencies, few iterations are necessary to determine the post-contingency maximum loading point. Thus, a significant reduction in the global number of iterations is achieved. Therefore, the proposed methodology can be used as an alternative technique to verify and even to obtain the list of critical contingencies supplied by the electric power systems security analysis function. © 2013 Elsevier Ltd. All rights reserved.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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A stability-indication high performance liquid chromatographic method has been developed for the determination of norfloxacin in tablet dosage forms. Optimum separation was achieved in less than 7 minutes using Eclipse Plus Zorbax C18 Agilent, 150 mm×4.6 mm i.d., 5 μm particle size column. The analyte was resolved by using a mobile phase 5% acetic acid aqueous solution and methanol (80:20, v/v) at a flow rate 1.0 ml/min on an isocratic high performance liquid chromatographic system at a wavelength of 277 nm. Linearity, system suitability, precision, sensitivity, selectivity, specific, and robustness were established by International Conference Harmonization guidelines. For stress studies the drug was subjected to photolysis, oxidation, acid, alkaline and neutral conditions. The analytical conditions and the solvent developed provided good resolution within a short analysis time and economic advantages. The proposed method not required sophisticated and expensive instrumentation.
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This paper describes a rapid method for arsenic (As) speciation by LC-ICP-MS in several types of food samples. Prior to analysis, samples were milled and the As species extracted from biological tissues by sonication in only 2 min with a solution containing MeOH (10%, v/v) plus HNO3 (2%, v/v). As species were separated by LC using an anion exchange column. Method detection limits for AsB, As3+,DMA, MMA and As5+ were 1.3, 0.9, 0.6, 0.7 and 0.8 ng g(-1), respectively. Method accuracy and precision were traceable to Certified Reference Materials SRM1577 bovine liver from the National Institute of Standards and Technology, CE278 mussel tissue from the Institute of Reference Materials and Measurements and DOLT-3 dogfish liver tissue and DORM-3 fish protein from the National Research Council of Canada. Finally, the method was applied to speciate As in food samples (egg, fish muscle, beef and chicken) purchased in Brazilian markets.