219 resultados para analytical method validation
Resumo:
An analytical method is proposed to study the attitude stability of a triaxial spacecraft moving in a circular Keplerian orbit in the geomagnetic field. The method is developed based on the electrodynamics effect of the influence of the Lorentz force acting on the charged spacecraft's surface. We assume that the rigid spacecraft is equipped with an electrostatic charged protective shield, having an intrinsic magnetic moment. The main elements of this shield are an electrostatic charged cylindrical screen surrounding the protected volume of the spacecraft. The rotational motion of the spacecraft about its centre of mass due to torques from gravitational force, as well Lorentz and magnetic forces is investigated. The equilibrium positions of the spacecraft in the orbital coordinate system are obtained. The necessary and sufficient conditions for the stability of the spacecraft's equilibrium positions are constructed using Lyapunov's direct method. The numerical results have shown that the Lorentz force has a significant influence on the stability of the equilibrium positions, which can affect the attitude stabilization of the spacecraft. (C) 2007 COSPAR. Published by Elsevier Ltd. All rights reserved.
Resumo:
In this report an analytical method to determine furosemide by using diffuse reflectance spectroscopy is presented. This study shows that this technique can give quantitative results using spot test analysis, particularly in the case of pharmaceuticals containing furosemide. The color spot test could be obtained by reaction between furosemide with p-dimethylaminocinnamaldehyde, in acid medium. This reaction produced a stable complex on filter paper after heating to 80degreesC for 5 min. All reflectance measurements were carried out at 585 nm and the linear range was from 7.56 x 10(-3) to 6.05 x 10(-2) mol l(-1), with a correlation coefficient of 0.999. The limit of detection was estimated to be 2.49 x 10(-3) mol l(-1) (R.S.D. = 1.7%) and the effect of common excipients on the reflectance measurements was evaluated. The method was applied to determine furosemide in commercial brands of pharmaceuticals. The results obtained by the proposed method were favorably compared with those of the official method, showing for the first time ever that quantitative spot test analysis by diffuse reflectance could be successfully used to determine furosemide in tablets. (C) 2004 Elsevier B.V. All rights reserved.
Resumo:
The Indanthrene Olive Green B (C.I. Vat Green 3; C.I. 69500), VG3 dye, a vat dye bearing an anthraquinonoid group and a ketonic group, can be detected by differential pulse voltammetry in alkaline solution using glassy carbon electrode. on the adsorbed form the dyes are reduced into three cathodic steps at -0.54 V, -0.65 V and -0.93 V vs Ag/AgCl. The leuco form generated after previous electrolysis at controlled potential of -1 V can be detected by voltammetry due to its reoxidation peak at -0.08 V. An analytical method is proposed for determining the vat dye using modified glassy carbon electrode by electrochemical activation in alkaline medium. Linear relationship was observed between l(Pu) vs concentration from I X 10(-5) mol L-1 to 6.0 X 10(-4) mol L-1. The detection limit was calculated to be 9.3 X 10(-6) mol L-1. (c) 2005 Elsevier Ltd. All rights reserved.
Resumo:
A rapid and efficient analytical method is presented for the quantitative analysis of 10 organochlorine pesticides in corn meal. The extraction and clean up steps are combined into one step by transferring the sample to a chromatographic column prepacked with alumina and silica gel. The pesticides are eluted with n-hexane-dichloromethane 9:1 (v/v) and the extracts analized by gas-liquid chromatography with electron capture detection, the average recoveries were between 78% and 98% and the detection limits were between 1 and 5 ng/g.
Resumo:
An efficient analytical method is described for the analysis of dicofol residues in pulp and orange peel. Samples are mixed with Celite and transferred to chromatographic columns prepacked with silica gel. Dicofol is eluted with ethyl acetate, and the extracts are analyzed by gas chromatography with electron capture detection. Mean recoveries for dicofol at levels of 0.5, 2.0, 5.0, and 10 mg/kg ranged from 87 to 95% with relative standard deviation values between 2.6 and 9.0%. To investigate the effect of a pilot washing system on dicofol residues in oranges, the analytical procedure was applied to samples submitted to different treatments with commercial formulations under field and laboratory conditions. The orange samples with and without washing were analyzed in duplicate, and the results indicated that washing under the described conditions did not allow a complete removal of dicofol residues from orange peel.
Resumo:
Prussian blue [PB, iron(III) hexacyanoferrate(II)] films are effective for the electrocatalysis of the persulfate (peroxodisulfate)/sulfate redox system. This has been exploited in the voltammetric determination of persulfate anions using a PB-modified platinum disc electrode. A linear correlation between electrocatalytic current and persulfate concentration was found for the range 5 x 10(-5) to 3 x 10(-3) mol dm(-3), using 0.100 mol dm(-3) potassium chloride as supporting electrolyte at pH 4. This analytical method has the advantages of speed and ease of operation in relation to traditional titrimetric methods for persulfate determination. The applicability of the method to the determination of persulfate in a commercial hair bleaching 'booster' product is demonstrated. (C) 2000 Elsevier B.V. B.V. All rights reserved.
Resumo:
This work presents a methodology for elastic-plastic fracture reliability analysis of plane and axisymmetric structures. The structural reliability analysis is accomplished by means of the FORM analytical method. The virtual crack extension technique based on a direct minimization of potencial energy is utililized for the calculation of the energy release rate. Results are presented to illustrate the performance of the adopted methodology.
Resumo:
A specific and sensitive high-performance liquid chromatographic procedure was developed for the assay of sparfloxacin in raw material and tablets. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay. The method validation yielded good results and included the range, linearity, precision, accuracy, specificity and recovery. This method can also be applied to stability studies. (C) 1999 Elsevier B.V. B.V. All rights reserved.
Resumo:
Alcohol dehydrogenases (ADHs) are oxidoreductases present in animal tissues, plants, and microorganisms. These enzymes attract major scientific interest for the evolutionary perspectives, afforded by their wide occurrence in nature, and for their use in synthesis, thanks to their broad substrate specificity and stereoselectivity. In the present study, the standardization of the activity of the alcohol dehydrogenase from baker's yeast was accomplished, and the pH and temperature stability showed, that the enzyme presented a high stability to pH 6.0-7.0 and the thermal stability were completely maintained up to 50 degrees C during 1 h. The assays of ethanol (detection range 1-5 mM or 4.6 x 10(-2) to 23.0 x 10(-2) g/L) in different samples in alcoholic beverages, presented a maximum deviation of only 7.2%. The standard curve and the analytic curve of this method meet the conditions of precision, sensitivity, simplicity, and low cost, required for a useable analytical method. (c) 2006 Elsevier B.V. All rights reserved.
Resumo:
A simple method was developed for the determination of fluquinconazole, pyrimethanil, and clofentezine in whole fruit; peel; and pulp of mango, apple, and papaya. These compounds were extracted from fruit samples with a mixture of ethyl acetate-n-hexane (1 + 1, v/v). An aliquot (2 mL) of the extract was evaporated to near dryness under a stream of nitrogen, and the residue was dissolved with 2 mL methanol. The analysis was performed by means of liquid chromatography with ultraviolet detection at 254 nm using a gradient solvent system. The method was validated with fortified fruit samples at concentration levels of 0.05, 0.10, 0.20, and 0.50 mg/kg. Average recoveries (4-8 replicates) ranged from 80 to 95% with relative standard deviations between 3.5 and 12.7%. Detection limits ranged from 0.03 to 0.05 mg/kg for fruit pulp and 0.03 mg/kg for whole fruit. The quantitation limits ranged from 0.05 to 0.10 mg/kg for fruit pulp and 0.05 mg/kg for whole fruit. The analytical method was applied to fruit samples obtained from local markets.
Resumo:
This work describes a novel approach for the analysis of selected aldehydes (formaldehyde, acetaldehyde, propionaldehyde, and acrolein) and acetone in environmental samples using micellar electrokinetic chromatography (MEKC). The method is based on the reaction of carbonyl compounds with 3-methyl-2-benzothiazoline hydrazone (MBTH) that gives an azine intermediate with maximum absorbance at 216 nm. A systematic evaluation of sample dissolution medium was conducted as a means to enhancing sensitivity. In the best condition, samples were dissolved in 0.030 mol.L-1 tetraborate solution. This condition presented enhancement factors in the range of 35-54 for the aldehydes under investigation, computed as the improvement of the concentration limits of detection (LODs) with reference to the sample dissolved in pure water. The running buffer was 0.020 mol.L-1 tetraborate, pH 9.3, containing 0.050 mol-L-1 sodium dodecyly sulfate (SIDS). The overall methodology presented several advantages over established methods for aldehydes. Worthy mentioning that MBTH is available in high purity degree, dispensing laborious reagent purification procedures. A few method validation parameters were determined revealing good migration time repeatability (< 2.5% coefficient of variation, CV) and area repeatability (< 4% CV), excellent linearity (20-120 mug/L, r > 0.995) and adequate sensitivity for environmental applications. The LODs with respect to each single aldehyde were in the range of 0.54-4.0 mug.L-1 and 11 mug.L-1 for acetone. The methodology was applied to the determination of aldehydes indoors. Samples were collected in an impinger flask containing 0.05% MBTH solution, at a flow rate of 0.80 L.min(-1), during 2.5 h, at different times during the day. The most abundant carbonyls in the samples were acetone, followed by formaldehyde and acetaldehyde, with estimate peak concentrations of 452, 5.2 and 2.2 ppbv, respectively.
Resumo:
An analytical method for the determination of aldicarb, and its two major metabolites, aldicarb sulfoxide and aldicarb sulfone in fruits and vegetables is described. Briefly the method consisted of the use of a methanolic extraction, liquid-liquid extraction followed by solid-phase extraction clean-up. Afterwards, the final extract is analyzed by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (LC-APCI-MS). The specific fragment ion corresponding to [M-74](+) and the protonated molecular [M+K](+) ion were used for the unequivocal determination of aldicarb and its two major metabolites. The analytical performance of the proposed method and the results achieved were compared with those obtained using the common analytical method involving LC with post-column fluorescence detection (FL). The limits of detection varied between 0.2 and 1.3 ng but under LC-FL were slightly lower than when using LC-APCI-MS. However both methods permitted one to achieve the desired sensitivity for analyzing aldicarb and its metabolites in vegetables. The method developed in this work was applied to the trace determination of aldicarb and its metabolites in crop and orange extracts. (C) 2000 Elsevier B.V. B.V. All rights reserved.
Resumo:
The purpose of this paper is to analyze the challenges to Political Sciences at the moment when many authors emphasize the usage of democratic paradigm as the only way to the rational building of speech in pluralist societies. At the end of one century of the consolidation of modern liberal thought, both in right and left versions (Wallerstein, 1995), the democracy as research tradition(Ball, 1987) fades away its ethical meaning, based upon equality and freedom, and lacks room for discussions about rules for implementing it. The analytical method seeks to historically rebuild the different levels of modern state-nation upbringing and the consolidation of competitive party democracy in the 20th century, which is the explanation key for the political organizational phenomenon of globalized societies. The result of this analysis opens new perspectives to Political Sciences advance in discussing the nature of democratic paradigm since it needs to face challenges to survive, such as: the fight against the structural violence of our society; the fight against despotism; and the adjustment to the meaning of the word freedom. The facing of the mentioned challenges may open explanation keys that will lead to a change in Political Sciences ways.
Resumo:
An inexpensive, simple, precise and rapid method for the determination of fluoroquinolone gatifloxacin in tablets is described. The procedure is based on the use of volumetric dosage in a non-aqueous medium in glacial acetic acid with 0.1 M perchloric acid. The method validation yielded good results and included the precision, recovery and accuracy. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay.
Resumo:
The present paper studies a system comprised of two blocks connected by springs and dampers, and a DC motor with limited power supply fixed on a block, characterizing a non-ideal problem. This DC motor exciting the system causes interactions between the motor and the structure supporting it. Because of that, the non-ideal mathematical formulation of the problem has one and a half extra degree of freedom than the ideal one. A suitable choice of physical parameters leads to internal resonance conditions, that is, its natural frequencies are multiple of each other, by a known integer quantity. The purpose here is to study the dynamic behavior of the system using an analytical method based on perturbation techniques. The literature shows that the averaging method is the more flexible method concerning non-ideal problems. Summarizing, an steady state solution in amplitude and phase coordinates was obtained with averaging method showing the dependence of the structure amplitudes with the rotation frequency of the motor. Moreover, this solution shows that on of the amplitude coordinates has influence in the determination of the stationary rotation frequency. The analytical solution obtained shows the presence of the rotation frequency in expressions representing the oscillations of the structure, and the presence of amplitude coordinates in expressions describing the dynamic motion of the DC motor. These characteristics show the influence not only of the motor on structure but also of the response of the structure on dynamical behavior of the motor. Copyright © 2005 by ASME.