48 resultados para Methods: analytical


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The chemical properties of 12 different peats have been analyzed by methods from VDLUFA (German Association of Agricultural Analysis and Research Institutes) and EN (European Committee for Standardization, Technical Committee 223: Soil improvers and growing media). The analyses of pH (CaCl 2), contents of salts (H 2O), nutrients (CAT), and Na and Cl (H 2O) were carried out by VDLUFA methods, while those of pH (H 2O), EC (H 2O), nutrients (CAT), Na (CAT and H 2O) and Cl (H 2O) according to EN. Ten milled or sod white peats and two dredged frozen black peats of different degrees of decomposition were used. All of them contained high amounts of Mg, while black peats were additionally high in N, Fe and Zn. The pH-values were about the same for all peats. N- and Mn-contents depended most on peat origin. Analytical values of both CAT-methods were in the same range. Extraction with H 2O (EN) as compared to CAT (EN) resulted in considerably lower values.

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The intension of this paper was to review and discuss some of the current quantitative analytical procedures which are used for quality control of pharmaceutical products. The selected papers were organized according to the analytical technique employed. Several techniques like ultraviolet/visible spectrophotometry, fluorimetry, titrimetry, electroanalytical techniques, chromatographic methods (thin-layer chromatography, gas chromatography and high-performance liquid chromatography), capillary electrophoresis and vibrational spectroscopies are the main techniques that have been used for the quantitative analysis of pharmaceutical compounds. In conclusion, although simple techniques such as UV/VIS spectrophotometry and TLC are still extensively employed, HPLC is the most popular instrumental technique used for the analysis of pharmaceuticals. Besides, a review of recent works in the area of pharmaceutical analysis showed a trend in the application of techniques increasingly rapid such as ultra performance liquid chromatography and the use of sensitive and specific detectors as mass spectrometers.

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The phases of a transmission line are tightly coupled due to mutual impedances and admittances of the line. One way to accomplish the calculations of currents and voltages in multi-phase lines consists in representing them in modal domain, where its n coupled phases are represented by their n propagation modes. The separation line in their modes of propagation is through the use of a modal transformation matrix whose columns are eigenvectors associated with the parameters of the line. Usually, this matrix is achieved through numerical methods which does not allow the achievement of an analytical model for line developed directly in the phases domain. This work will show the modal transformation matrix of a hypothetical two-phase obtained with numerical and analytical procedures. It will be shown currents and voltage s at terminals of the line taking into account the use of modal transformation matrices obtained by using numerical and analytical procedures. © 2011 IEEE.

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Chromatographic and electroanalytical methods were developed to detect and quantify Sudan II (SD-II) dye in fuel ethanol samples. Sudan II is reduced at +0.50 V vs. Ag/AgCl on a glassy carbon electrode using Britton-Robinson buffer (pH 4.0) and N,N-dimethylformamide (70:30, v/v) + sodium dioctyl sulfosuccinate surfactant as supporting electrolyte, due to the azo group. This is the basis for its determination by square-wave voltammetry (SWV). Using the optimized conditions, it is possible to get a linear calibration curve from 3.00×10-6 to 1.80×10-5 mol L-1 (r = 0.998) with limits of detection (LOD) and quantification (LOQ) of 2.05×10-6 and 6.76×10-6 mol L-1, respectively. In addition, the hydroxyl substituent in the SD-II dye is also oxidized at +0.85 V vs. Ag/AgCl, which was conveniently used for its determination by high-performance liquid chromatography coupled to electrochemical detection (HPLC-ED). Under the optimized condition, the SD-II dye was eluted and separated using a reversed-phase column (cyanopropyl, CN) using isocratic elution with the mobile phase containing acetonitrile and aqueous lithium chloride (5.00×10-4 mol L-1) at 70:30 (v/v) and a flow rate of 1.2 mL min-1. Linear calibration curves were obtained from 3.00×10-7 to 2.00×10-6 mol L-1 (r = 0.999) with LOD and LOQ of 3.10×10-8 and 1.05×10-7 mol L-1, respectively. Both methods were simple, fast and suitable to detect and quantify the dye in fuel ethanol samples at recovery values between 83.0 to 102% (SWV) and 88.0 to 112% (HPLC-ED) with satisfactory precision and accuracy.

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The meta-analysis was used to evaluate the performance of piglets in post-weaning period, without imposition of sanitary challenge and fed diets containing blood plasma, obtained by spray-dried process (SDBP). Piglets are faced with normal challenges in post-weaning period such as environmental stress and the substitution of the liquid diet to a solid one. References regarding sanitary challenges were disregarded in this study. Only data regarding normal and expected challenges were considered. Data were obtained from indexed journals with information extracted from the material, methods and results sections of pre-selected scientific articles. First, the database was analyzed graphically to observe the distribution of data and presence of outliers. Afterwards correlation analysis and variance-covariance analyses were carried out. The database contained a total of 23 articles. The average initial weight of the piglets was 8.02. kg (4.00-9.28. kg) and the average initial age was 27 days (14-32 days). The average duration of feeding diets containing spray-dried blood plasma (SDBP) was 9 days (6-28 days). SDBP increased the feed conversion by 20.2% (P<0.05) during the initial period. Feed conversion during the total period was 10.2% higher (P<0.05) for animals fed with SDBP. Average daily weight gain and daily feed intake were not affected (P>0.05) during the entire period, but average daily gain was higher (P<0.05) for animals fed with SDBP during the initial period. The initial age of supplementation influenced the average daily weight gain and average daily feed intake of animals fed with SDBP. Better results were obtained than those obtained for animals up to 35 days of age fed diets without added SDBP supplementation. In early post-weaning period for piglets weaned up to 35 days of age, the SDBP supplementation positively influenced the average daily weight gain and feed conversion. © 2013 Elsevier B.V.

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Countries have different official programs and implement different sampling methods for the detection of Salmonella on poultry carcasses. In Brazil, a 25-g sample of skin and muscle excision (SME) from the wings, neck, and pericloacal parts is used; in the European Union (EU), a 25-g sample of neck skin (NSE) is used; and, in the United States, the whole carcass is rinsed with 400 ml of diluent (WCR). In the present study, these methods were evaluated to compare Salmonella occurrence and counts of hygiene indicator microorganisms (Escherichia coli, Enterobacteriaceae, and total viable count of aerobic mesophilic bacteria) using different carcasses from the same flock and also using different analytical units taken from the same carcass. Eighty flocks, with four broiler carcasses from each, were included in this study; three broilers were sampled according to protocols from Brazil, the EU, and the United States, and the last one by all three methods. SME, NSE, and WCR provided equivalent results (P > 0.05) for Salmonella detection on broiler carcasses when using different carcasses from the same flock and when using the same carcass. The predominant serovar was Salmonella Enteritidis. For the enumeration of hygiene indicator microorganisms, WRC provided higher counts than SME or NSE (P < 0.05), when using both the same or different carcasses. Therefore, it is possible to directly compare Salmonella results in poultry carcasses when using the methods recommended by the legislative bodies of Brazil, the United States, and the EU. However, WCR provides the best results for hygiene indicator microorganisms. Copyright © International Association for Food Protection.

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CONTEXTO E OBJETIVO:Há poucos estudos sobre os fatores de risco para os subgrupos de gagueira. O objetivo deste estudo foi caracterizar os fatores de risco para a gagueira desenvolvimental familial em meninos que gaguejam e que não gaguejam como tipologia das disfluências, fatores qualitativos e comunicativos associados, estresse físico e emocional, atitude familiar e reação pessoal.TIPO DE ESTUDO E LOCAL:Estudo transversal analítico com um grupo controle, realizado no Laboratório de Estudo da Fluência, que faz parte do Departamento de Fonoaudiologia de uma universidade pública.MÉTODOS:Pais de 40 meninos com e sem gagueira pareados por idade fizeram parte do estudo. Os participantes foram divididos em dois grupos: crianças com gagueira e crianças sem gagueira, com idades entre 6 anos 0 meses e 11 anos 11 meses Inicialmente todos os participantes foram submetidos a uma avaliação de fluência e depois os dados foram coletados por meio do Protocolo de Risco para a Gagueira do Desenvolvimento.RESULTADOS:Não foi observada diferença nos fatores de estresse físicos e reações pessoais entre os grupos. As atitudes inadequadas familiares foram apresentadas por 95% das crianças com gagueira e 30% das crianças sem gagueira. Quatro fatores de risco analisados não ocorreram nas crianças sem gagueira, a saber, disfluências gagas, fatores qualitativos, estresse físico e emocional.CONCLUSÕES:Os achados sugerem que a presença de disfluências gagas, fatores qualitativos e comunicativos associados, estresse emocional e atitude familiar inadequada são fatores de risco importantes para a gagueira desenvolvimental familial em meninos.

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Because the biomechanical behavior of dental implants is different from that of natural tooth, clinical problems may occur. The mechanism of stress distribution and load transfer to the implant/bone interface is a critical issue affecting the success rate of implants. Therefore, the aim of this study was to conduct a brief literature review of the available stress analysis methods to study implant-supported prosthesis loading and to discuss their contributions in the biomechanical evaluation of oral rehabilitation with implants. Several studies have used experimental, analytical, and computational models by means of finite element models (FEM), photoelasticity, strain gauges and associations of these methods to evaluate the biomechanical behavior of dental implants. The FEM has been used to evaluate new components, configurations, materials, and shapes of implants. The greatest advantage of the photoelastic method is the ability to visualize the stresses in complex structures, such as oral structures, and to observe the stress patterns in the whole model, allowing the researcher to localize and quantify the stress magnitude. Strain gauges can be used to assess in vivo and in vitro stress in prostheses, implants, and teeth. Some authors use the strain gauge technique with photoelasticity or FEM techniques. These methodologies can be widely applied in dentistry, mainly in the research field. Therefore, they can guide further research and clinical studies by predicting some disadvantages and streamlining clinical time.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Chemical degradation of drugs may result in altered therapeutic efficacy and even toxic effects. Therefore, understanding the factors that change the stability of pharmaceuticals and identifying ways to guarantee their stability are important. In this work stability-indicating Liquid Chromatographic (LC) and bioassay methods were validated and employed in the fluconazole stability studies. The correlation of sample results from both methods was evaluated. Fluconazole raw material stability was investigated in aqueous, acid (0.1 M HCl), alkaline (0.1 M NaOH) and oxidative (3% v/v H2O2) reflux for 6 hours, by LC method. Fluconazole capsules were exposed to UVC (254 nm, 66 and 180 days), climatic chamber (40°C, 75% RH, 90 days) and oven (60°C, 60 days), these samples were analyzed by LC and bioassay methods It was found that the drug is degraded (10% decrease) with arising of a possible degradation product in an oxidative medium and UVC exposure, in all the others conditions fluconazole remained chemically stable (higher than 98%) when analyzed by LC. However when the capsules stressed samples were evaluated through bioassay very low antifungal activity was found (about 30%). Fluconazole showed to be an unstable drug and it indicates that special care must be taken during the handling, storage and quality control using appropriated methods to analyze this therapeutic agent. This work suggests monitoring the fluconazole stability by bioassay and the stability-indicating LC methods.

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Sodium azumolene is a drug designed to fight Malignant Hyperthermia (MH), which is characterized by genetic predisposition and triggered by the use of inhalational anesthetics. This drug is shown as a water-soluble analogue of dantrolene sodium, 30-folds more water soluble, which gives advantages for its emergency use. To our knowledge there is no analytical method for sodium zaumolene raw material or dosage form published so far. The objective of the present investigation was to develop and validate analytical methods to achieve sodium azumolene chemical identification and quantification. The sodium azumolene was characterized regarding its thermal behavior, by differential thermal analysis and thermogravimetric analysis; Visible, UV and infrared absorption. To accurately assess the sodium Azumolene content three different analytical methods (visible and UV spectrophotometry and high performance liquid chromatography) were developed and validated. All methods showed to be linear, accurate, precise and reliable. Azumolene has shown to be equipotent to dantrolene in the treatment and prevention of an MH crisis and the great advantage compared to dantrolene is better water solubility. This study has characterized the sodium azumolene and presents new analytical methods which have not been reported so far.

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Darunavir, a protease inhibitor used in the treatment of HIV infection, presents few methods for its determination in pharmaceuticals. Infrared (IR) spectroscopy offers the possibility of obtaining spectra relatively quickly, providing interesting information, analytically, qualitatively or quantitatively. Capillary electrophoresis (CE) performs separations of high efficiency in shorter time with reagents and samples in small quantity. These two methods are cost-benefitted when we evaluate the green level and the cost of analysis. Faster and cheaper methods without generating organic waste by IR and CE for the quantification of darunavir were developed and validated, focusing socioeconomic impact of analytical decisions. If the cost of acquisition, maintenance, production, analysis and conditioning of drugs and pharmaceuticals is high, consequently the price of this product in the market will be higher and it cannot be accessible to the patient. Treatment failure not only affects the quality of life of patients, but also contributes significantly to the economic burden of the health system. In this context there is a tool called Analysis of the Life Cycle, which comes to make us think in a multidimensional way focusing the whole, the parts and especially the interaction among the parts of a system.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)