999 resultados para validação analítica


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Due necessity of better understanding leptin and reproduction relations, a specific radioimmunoassay (RIA) to bovine leptin was avalidated. First, an antibody production protocol was developed using recombinant equine leptin inoculated in a rabbit, that results in 28,05% of maximum binding (MB) 105 days after the protocol beginning. The tests of validations verified parallelism between standard curve and dilutions of high and low controls (P < 0,01). Antibody against equine leptin showed specificity to bovine leptin (P < 0,01). The recuperation tax of bovine leptin by antibody against recombinant equine leptin was from 98,4 to 101,6% (P < 0, 01). When the samples were stored in ambient temperature or refrigerated to 4°C, ligation stability was verified (P > 0,2), however, temperatures above 37°C impaired the bovine leptin recuperation. The use of assay buffer with or without bovine plasma did not show any difference (P > 0,3). These results showed that the antibody produced in rabbit against equine leptin were able to detect plasmatic bovine leptin, and that the RIA to bovine leptin quantification had adequate characteristics to the development of a valid assay.

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Triamcinolone (TRI), a drug widely used in the treatment of ocular inflammatory diseases, is practically insoluble in water, which limits its use in eye drops. Cyclodextrins (CDs) have been used to increase the solubility or dissolution rate of drugs. The purpose of the present study was to validate a UV-Vis spectrophotometric method for quantitative analysis of TRI in inclusion complexes with beta-cyclodextrin (B-CD) associated with triethanolamine (TEA) (ternary complex). The proposed analytical method was validated with respect to the parameters established by the Brazilian regulatory National Agency of Sanitary Monitoring (ANVISA). The analytical measurements of absorbance were made at 242nm, at room temperature, in a 1-cm path-length cuvette. The precision and accuracy studies were performed at five concentration levels (4, 8, 12, 18 and 20μg.mL -1). The B-CD associated with TEA did not provoke any alteration in the photochemical behavior of TRI. The results for the measured analytical parameters showed the success of the method. The standard curve was linear (r2 > 0.999) in the concentration range from 2 to 24 μg.mL -1. The method achieved good precision levels in the inter-day (relative standard deviation-RSD <3.4%) and reproducibility (RSD <3.8%) tests. The accuracy was about 80% and the pH changes introduced in the robustness study did not reveal any relevant interference at any of the studied concentrations. The experimental results demonstrate a simple, rapid and affordable UV-Vis spectrophotometric method that could be applied to the quantitation of TRI in this ternary complex.

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Objective: To characterize physically and chemically, non-sweetened orange juices and orange nectars sweetened with sucrose or sweet flavoring agents, with respect to their pH, titratable acidity (TA) and total soluble solids content (TSSC), as well as to evaluate the correlation of the latter property with the others. Method: Aliquots of three lots of two orange juices and two orange nectars containing sucrose and two containing sweet flavoring agents were evaluated. Mineral water was used as a control. The TSSC was determined using an Abbe refractometer. The pH was recorded using a digital pH meter, while TA was quantified by titrating samples of the beverages with 0.1 M NaOH until reaching pHs 5.5 and 7.0. Data were subjected to Pearson's correlation test, regression analysis, analysis of variance and Tukey's test (α=0.05). Results: TSSC values presented a strong correlation with TA, and these properties exhibited a quadratic relationship. Although the pH values were not dependent on the presence of sucrose or sweet flavoring agents, a significantly greater amount of base was necessary to reach pHs 5.5 and 7.0 in the beverages without sucrose or flavoring agents. Conclusion: Orange juices and nectars presented similar pH values, which was not associated with the presence of sucrose or sweet flavoring agents in the beverages. Higher TA values were obtained for the juice and lower for the nectars, regardless of containing sucrose or sweet flavoring agents. The increase of TSSC did not implicate in decrease of TA in the beverages.

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Pós-graduação em Alimentos e Nutrição - FCFAR

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Pós-graduação em Ciências Cartográficas - FCT