744 resultados para hydroxylamine hydrochloride derivatization


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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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This paper describes an analytical reflectometric method that has an objective not only the industrial quality control but also to detect possible falsifications and/or adulterations of propranolol in pharmaceutical formulations. The method is based on the diffuse reflectance measurements of the colored product (III) of the spot test reaction between propranolol hydrochloride (I) and 2,6-dichloroquinone-4-chloroimide (II) using filter paper as solid support. Spot test conditions have been investigated using experimental design in order to identify and optimize the critical factors. The factors evaluated were DCQ concentration, propranolol solvent and DCQ solvent. The best reaction conditions were achieved with the addition of 30 mu L, of propranolol solution in ethanol 35% (v/v) and 30 mu L of DCQ solution at 70 mg mL(-1) in acetone, in this order. All reflectance measurements were carried out at 500 nm and the linear range was from 8.45 x 10(-4) to 8.45 x 10(-2) mol L-1 (r= 0.998). The limit of detection was 1.01 x 10(-4) mol L-1. No interference was observed from the assessed excipients and drugs. The method was applied to determine propranolol in commercial brands of pharmaceuticals. The results obtained by the proposed method were favorably compared with those given by the British Pharmacopoeia procedure. (C) 2007 Elsevier B.V. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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This paper provides a review on the latest advances and applications of the luminescence spectroscopy for the development of pharmaceuticals analyses methods, basically based on the photo- and chemiluminescence. The different forms of the drugs determination on pharmaceuticals through the fluorescence and chemiluminescence are discussed. The analyses include the drugs native fluorescence (liquid and solid-phases); the fluorescence from the oxidizing or reducing forms of the drug; the fluorescence from the chemical derivatization and their photochemistry and hydrolysis reactions. The quenching of luminescence and chemiluminescence generation for the pharmaceutical quantification are also shown. Finally, the trends and future perspectives of the luminescence spectroscopy in the field of the pharmaceutical research are discussed.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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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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A case admitted at the Small Animals Clinics Service, Veterinary Hospital, FMVZ - UNESP, in May, 1999 is described. A Brazilian Terrier dog, 3 years and 3 months old, weighing 1.7 kg was brought after 2 hours and a half from contact with a scorpion (Tityus bahiensis). The dog showed vocalization inserted with drowsiness. Physical examination showed slightly hyperemic mucous, pain, agressiveness, tachypnea, tachycardia, and discrete erythema on the right forelimb palmar face. An anesthetic block was performed around the stung area using 2% lidocaine hydrochloride without vasoconstrictor (10mL). The animal was asymptomatic, after 24 h treatment.

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Electroactive films of iron tetrasulfonated phthalocyanine (FeTsPc) were assembled via the electrostatic layer-by-layer technique (LBL), in which FeTsPc layers were alternated with the polycationic poly(allylamine hydrochloride) (PAN). The multilayer formation was monitored via UV-Vis spectroscopy by measuring the increase in the Q Band of FeTsPc at 676 nm. Film thickness was estimated by profilometry as ca. 10 Angstrom per bilayer. Fourier transform infrared and UV-Vis absorption spectroscopy suggested specific interactions between FeTsPc and PAR Cyclic voltammograms showed reproducible pairs of oxidation-reduction peaks at 0.92 mV and 0.70 mV, respectively, for a 50-bilayer PAH/FeTsPc film at 50 mV/s (vs Ag/AgNO3).

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A rapid and simple method for procaine determination was developed by flow injection analysis (FIA) using a screen-printed carbon electrode (SPCE) as amperometric detector. The present method is based on the amine/hydroxylamine oxidation from procaine monitored at 0.80 V on SPCE in sodium acetate solution pH 6.0. Using the best experimental conditions assigned as: pH 6.0, flow rate of 3.8 mL min(-1), sample volume of 100 mu L and analytical path of 30 cm it is possible to construct a linear calibration curve from 9.0 x 10(-6) to 1.0 x 10(-4) mol L-1. The relative standard deviation for 5.0 x 10(-5) mol L-1 procaine (15 repetitions using the same electrode) is 3.2% and detection limit calculated is 6.0 x 10(-6) mol L-1. Recoveries obtained for procaine gave a mean values from 94.8 to 102.3% and an analytical frequency of 36 injections per hour was achieved. The method was successfully applied for the determination of procaine in pharmaceutical formulation without any pre-treatment, which are in good accordance with the declared values of manufacturer and an official method based on spectrophotometric analysis. (c) 2006 Elsevier B.V. All rights reserved.