52 resultados para Method of quantification


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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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A simple, rapid and sensitive spectrophotometric method has been developed for the determination of methyldopa in pharmaceutical formulations. The method is based on the reaction between tetrachloro-p-benzoquinone (p-chloranil) and methyldopa, accelerated by hydrogen peroxide (H 2O 2), producing a violet-red compound (λmax = 535 nm) at ambient temperature (25.0 ± 0.2°C). Experimental design methodologies were used to optimize the measurement conditions. Beer's law is obeyed in a concentration range from 2.10 × 10 -4 to 2.48 × 10 -3 mol L -1 (r = 0.9997). The limit of detection was 7.55 × 10 -6 mol L -1 and the limit of quantification was 2.52 × 10 -5 mol L -1. The intraday precision and interday precision were studied for 10 replicate analyses of 1.59 × 10 -3 mol L -1 methyldopa solution and the respective coefficients of variation were 0.7 and 1.1%. The proposed method was successfully applied to the determination of methyldopa in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95% confidence level.

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Lubricating oils are crucial in the operation of automotive engines because they both reduce friction between moving parts and protect against corrosion. However, the performance of lubricant oil may be affected by contaminants, such as gasoline, diesel, ethanol, water and ethylene glycol. Although there are many standard methods and studies related to the quantification of contaminants in lubricant oil, such as gasoline and diesel oil, to the best of our knowledge, no methods have been reported for the quantification of ethanol in used Otto cycle engine lubrication oils. Therefore, this work aimed at the development and validation of a routine method based on partial least-squares multivariate analysis combined with attenuated total reflectance in the mid-infrared region to quantify ethanol content in used lubrication oil. The method was validated based on its figures of merit (using the net analyte signal) as follows: limit of detection (0.049%), limit of quantification (0.16%), accuracy (root mean square error of prediction=0.089% w/w), repeatability (0.05% w/w), fit (R 2 =0.9997), mean selectivity (0.047), sensitivity (0.011), inverse analytical sensitivity (0.016% w/w-1) and signal-to-noise ratio (max: 812.4 and min: 200.9). The results show that the proposed method can be routinely implemented for the quality control of lubricant oils. © 2013 Elsevier B.V. All rights reserved.

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