84 resultados para Optimized using

em Repositório Institucional UNESP - Universidade Estadual Paulista "Julio de Mesquita Filho"


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A flow-injection (FI) spectrophotometric procedure exploiting merging zones is proposed for the determination of azithromycin in pharmaceutical formulations. The method is based on the reaction of azithromycin with tetrachloro-phenzoquinone (p-chloranil) accelerated by hydrogen peroxide and conducted in a methanol medium, producing a purple-red color compound (lambda(max) = 540 nm). The FI system and the experimental conditions were optimized using a multivariate method. Beer's law is obeyed in a concentration range of 50 - 1600 mu g mL(-1) with an excellent correlation coefficient (r = 0.9998). The detection limit and the quantification limit were 6.6 and 22.1 mu g mL(-1), respectively. No interference was observed from the common excipients, and the recoveries were within 98.6 to 100.4%. The procedure was applied to the determination of azithromycin in pharmaceuticals with a high sampling rate (65 samples h(-1)). The results obtained by the proposed method were in good agreement with those obtained by the comparative method at 95% confidence level.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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This work proposes a spectrophotometric method for the determination of hydrogen peroxide during photodegradation reactions. The method is based on the reaction of H2O2 with amonium metavanadate in acidic medium, which results in the formation of a red-orange color peroxovanadium cation, with maximum absorbance at 450 nm. The method was optimized using the multivariate analysis providing the minimum concentration of vanadate (6.2 mmol L-1) for the maximum absorbance signal. Under these conditions, the detection limit is 143 mu mol L-1. The reaction product showed to be very stable for samples of peroxide concentrations up to 3 mmol L-1 at room temperature during 180 h. For higher concentrations however, samples must be kept refrigerated (4 degrees C) or diluted. The method showed no interference of Cl- (0.2-1.3 mmol L-1), NO3- (0.3-1.0 mmol L-1), Fe3+, (0.2-1.2 mmol L-1) and 2,4-dichlorophenol (DCP) (0.2-1.0 mmol L-1). When compared to iodometric titration, the vanadate method showed a good agreament. The method was applied for the evaluation of peroxide consumption during photo-Fenton degradation of 2,4-dichlorophenol using blacklight irradiation. (c) 2004 Elsevier B.V. All rights reserved.

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A solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica (SiAt-SPCPE) was applied to Ni2+ determination in commercial ethanol fuel samples. The proposed method comprised four steps: (1) Ni2+ preconcentration at open circuit potential directly in the ethanol fuel sample, (2) transference of the electrode to an electrochemical cell containing DMG, (3) differential pulse voltammogram registering and (4) surface regeneration by polishing the electrode. The proposed method combines the high Ni2+ adsorption capacity presented by 2-aminothiazole organofunctionalized silica with the electrochemical properties of the Ni(DMG)2 complex, whose electrochemical reduction provides the analytical signal.All experimental parameters involved in the proposed method were optimized. Using a preconcentration time of 20 min, it was obtained a linear range from 7.5 x 10(-9) to 1.0 x 10(-6) mol L-1 with detection limit of 2.0 x 10(-9) mol L-1. Recovery values between 96.5 and 102.4% were obtained for commercial samples spiked with 1.0 mu mol L-1 Ni2+ and the developed electrode was totally stable in ethanolic solutions. The contents of Ni2+ found in the commercial samples using the proposed method were compared to those obtained by graphite furnace atomic absorption spectroscopy by using the F- and t-test. Neither the F- nor t-values exceeded the critical values at 95% confidence level, confirming that there are not statistical differences between the results obtained by both methods. These results indicate that the developed electrode can be successfully employed to reliable Ni2+ determination in commercial ethanol fuel samples without any sample pretreatment or dilution step. (c) 2006 Elsevier B.V. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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(1) C13H13N3O5, Mr = 291.26, P (1) over bar, a = 7.4629(9), b = 7.9203(9), c = 12.126(2) angstrom, alpha = 86.804(5), beta = 78.471(7), gamma = 69.401(8)degrees, V = 657.3(2)angstrom(3), Z = 2, R-1 = 0.0454; (2) C11H12N2O4, Mr=236.23, Pbca, a=7.2713(9), b=14.234(1), c=20.848(3)angstrom, V= 2157.8(4) angstrom(3), Z=8, R-1=0.0504; (3) C13H13N2O3Cl, Mr = 280.70, P2/n, a = 17.344(2), b = 9.237(1), c = 18.398(2) angstrom; beta = 92.61(2)degrees, V = 2944.4(6) angstrom(3), Z = 8, R-1 = 0.0714. The conformational features of three 4-substituted-3-4-dihydropyrimidin-2(1H)-ones were investigated by computational and single crystal X-ray crystallographic studies. The geometries were optimized using semiempirical (AM1) and first principle calculations (B3LYP/6-31G**) methods, the rotational barriers for important functional groups were studied. In all structures the pyrimidinone rings are in a more or less distorted boat conformation. The phenyl and the furane rings are almost perpendicular to the best least-squares plane through the dihydropyrimidinone ring.

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Hebanthe eriantha (Poir.) Pedersen (Amaranthaceae), which is known as Brazilian ginseng is widely used in folk medicine as an aphrodisiac and antidiabetic tonic. The anti-tumor activity, attributed to the pfaffic acid present in roots of H. eriantha, is responsible for the great interest in the commercialization of this species. In Brazil, the species H. eriantha is mainly used in commercial preparations, although other plants of the genus Pfaffia and Hebanthe have been marketed as Pfaffia paniculata or Brazilian ginseng. The pfaffic acid present in the roots is mainly conjugated with sugars (pfaffosides) and can be used as an active marker of H. eriantha, which helps to differentiate this species from others marketed as Brazilian ginseng. The main objective of this study was to develop and validate a liquid chromatographic method to quantify pfaffic acid in the roots of H. eriantha. The extraction and hydrolysis conditions were optimized using an univariate and experimental design, respectively, and the quantification of pfaffic acid by high performance liquid chromatography with diode-array detection (HPLC-DAD) was validated. This method was used to evaluate the pfaffic acid content in 30 different genotypes of the species from a germplasm collection. The content of pfaffic acid ranged from 0.97 to 4.29% (w/w) on a dry weight basis. © 2013 Elsevier B.V.

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This paper describes the development and application of a simple, cheap, and clean method for the quantification of furosemide in urine samples from athletes, to detect doping, using a combined spot test/diffuse reflectance spectroscopy procedure. The method is based on the complexation reaction of furosemide (5-(aminosulfonyl)-4-chloro-2-((furanylmethyl)amino)benzoic acid, dissolved in ethanol, with FeCl3 and the surfactant dodecyltrimethylammonium bromide (DTAB) in aqueous solution, yielding a colored compound on the surface of a filter paper. The reagent concentrations were optimized using a chemometric experimental design. The reflectometric measurements of the complex formed were carried out at 477nm. The linear range obtained was 1.65-9.00×10-3molL-1 of furosemide (R=0.997), and the detection and quantification limits were 4.9×10-4 and 1.62×10-3molL-1, respectively. The proposed method was successfully applied in the analysis of furosemide in spiked urine, demonstrating that it is a reliable alternative method for the detection of furosemide doping in sport. © 2012 Elsevier B.V..

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