260 resultados para bioanalytical method validation


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This article describes and discusses a method to determine root curvature radius by using cone-beam computed tomography (CBCT). The severity of root canal curvature is essential to select instrument and instrumentation technique. The diagnosis and planning of root canal treatment have traditionally been made based on periapical radiography. However, the higher accuracy of CBCT images to identify anatomic and pathologic alterations compared to panoramic and periapical radiographs has been shown to reduce the incidence of false-negative results. In high-resolution images, the measurement of root curvature radius can be obtained by circumcenter. Based on 3 mathematical points determined with the working tools of Planimp® software, it is possible to calculate root curvature radius in both apical and coronal directions. The CBCT-aided method for determination of root curvature radius presented in this article is easy to perform, reproducible and allows a more reliable and predictable endodontic planning, which reflects directly on a more efficacious preparation of curved root canals.

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OBJECTIVE: To assess microleakage in conservative class V cavities prepared with aluminum-oxide air abrasion or turbine and restored with self-etching or etch-and-rinse adhesive systems. Materials and Methods: Forty premolars were randomly assigned to 4 groups (I and II: air abrasion; III and IV: turbine) and class V cavities were prepared on the buccal surfaces. Conditioning approaches were: groups I/III - 37% phosphoric acid; groups II/IV - self-priming etchant (Tyrian-SPE). Cavities were restored with One Step Plus/Filtek Z250. After finishing, specimens were thermocycled, immersed in 50% silver nitrate, and serially sectioned. Microleakage at the occlusal and cervical interfaces was measured in mm and calculated by a software. Data were subjected to ANOVA and Tukey's test (α=0.05). RESULTS: Marginal seal provided by air abrasion was similar to high-speed handpiece, except for group I. There was SIGNIFICANT difference between enamel and dentin/cementum margins for to group I and II: air abrasion. The etch-and-rinse adhesive system promoted a better marginal seal. At enamel and dentin/cementum margins, the highest microleakage values were found in cavities treated with the self-etching adhesive system. At dentin/cementum margins, high-speed handpiece preparations associated with etch-and-rinse system provided the least dye penetration. CONCLUSION: Marginal seal of cavities prepared with aluminum-oxide air abrasion was different from that of conventionally prepared cavities, and the etch-and-rinse system promoted higher marginal seal at both enamel and dentin margins.

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The aim of this study was to assess the Knoop hardness of three high viscous glass ionomer cements: G1 - Ketac Molar; G2 - Ketac Molar Easymix (3M ESPE) and G3 - Magic Glass ART (Vigodent). As a parallel goal, three different methods for insertion of Ketac Molar Easymix were tested: G4 - conventional spatula; G5 - commercial syringe (Centrix) and G6 - low-cost syringe. Ten specimens of each group were prepared and the Knoop hardness was determined 5 times on each specimen with a HM-124 hardness machine (25 g/30 s dwell time) after 24 h, 1 and 2 weeks. During the entire test period, the specimens were stored in liquid paraffin at 37ºC. Significant differences were found between G3 and G1/G2 (two-way ANOVA and Tukey's post hoc test; p<0.01). There was no significant difference in the results among the multiple ways of insertion. The glass ionomer cement Magic Glass ART showed the lowest hardness, while the insertion technique had no significant influence on hardness.

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The mineralogical characterization through mineral quantification of Brazilian soils by X-ray diffraction data using the Rietveld Method is not common. A mineralogical quantification of an Acric Ferralsol from the Ponta Grossa region, state of Paraná, Brazil, was carried out using this Method with X-Ray Diffraction data to verify if this method was suitable for mineral quantification of a highly-weathered soil. The A, AB and B3 horizons were fractioned to separate the different particle sizes: clay, silt, fine sand (by Stokes Law) and coarse sand fractions (by sieving), with the procedure free of chemical treatments. X-ray Fluorescence, Inductively Coupled Plasma Atomic Emission Spectrometry, Infrared Spectroscopy and Mössbauer Spectroscopy were used in order to assist the mineral identification and quantification. The Rietveld Method enabled the quantification of the present minerals. In a general way, the quantitative mineralogical characterization by the Rietveld Method revealed that quartz, gibbsite, rutile, hematite, goethite, kaolinite and halloysite were present in the clay and silt fractions of all horizons. The silt fractions of the deeper horizons were different from the more superficial ones due to the presence of large amounts of quartz. The fine and the coarse sand fractions are constituted mainly by quartz. Therefore, a mineralogical quantification of the finer fraction (clay and silt) by the Rietveld Method was successful.

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An analytical procedure for determination of estriol, 17β-estradiol, estrone and 17α-ethinylestradiol in drinking water is presented. The method employs solid phase extraction (SPE) and sample dechlorination as cleanup procedures, followed by HPLC-DAD analysis. Validation was carried out using RE No. 899/2003 guidelines established by the Agência Nacional de Vigilância Sanitária (National Agency of Sanitary Surveillance, Brazil), with some adaptations. The statistically evaluated results have shown that the method is selective, precise (0,06% to 19,40% CV) and accurate (91,52% to 109,41% average recoveries). The developed method was applied to the analysis of these contaminants in drinking water from São Luís, MA.

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The increasing demand for fatty acid-free lecithin required modifications in existing purification methods. In this technical note we describe a purification procedure with the following steps: a) homogenization and extraction of yolks obtained from fresh eggs with acetone, b) solubilization with ethanol and solvent elimination and c) repeated solubilization/precipitation with petroleum ether/acetone. This crude extract was chromatographed on neutral alumina, which was exhaustively washed with chloroform before elution with chloroform:methanol, allowing the sequential separation of fatty acids and lecithin. Chromatographic behavior and mass spectra of the product are presented. This fast procedure yields fatty acid-free lecithin at a competitive cost.

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The aim of this study was to translate, validate and verify the reliability of the Body Area Scale (BAS). Participants were 386 teenagers, enrolled in a private school. Translation into Portuguese was conducted. The instrument was evaluated for internal consistency and construct validation analysis. Reproducibility was evaluated using the Wilcoxon test and the coefficient of interclass correlation. The BAS demonstrated good values for internal consistency (0.90 and 0.88) and was able to discriminate boys and girls according to nutritional state (p = 0.020 and p = 0.026, respectively). BAS scores correlated with adolescents' BMI (r = 0.14, p = 0.055; r = 0.23, p = 0.001) and WC (r =0.13, p = 0.083; r = 0.22, 0.002). Reliability was confirmed by the coefficient of inter-class correlation (0.35, p < 0.001; 0.60, p < 0.001) for boys and girls, respectively. The instrument performed well in terms of understanding and time of completion. BAS was successfully translated into Portuguese and presented good validity when applied to adolescents.

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OBJETIVO: Verificar a validade do Questionário de Freqüência Alimentar para Adolescentes para avaliar o consumo de grupos de alimentos entre escolares de Piracicaba, São Paulo. MÉTODOS: Participaram do estudo 94 adolescentes, com idade entre 11 e 15 anos, matriculados em uma escola da rede pública. O consumo alimentar foi avaliado pelo Questionário de Freqüência Alimentar para Adolescentes (QFAA) e a média de dois Recordatórios de 24 horas (R24h) foi utilizada como método de referência. Os itens alimentares foram classificados em 18 grupos. Foram realizadas análises descritivas, teste t-Student pareado e de Wilcoxon, coeficientes de correlação de Pearson e de Spearman. Foram também utilizadas análise de quartis e estatística Kappa ponderado. Os coeficientes de correlação foram corrigidos pela variância intrapessoal dos R24h, estimada a partir de ANOVA com um fator de classificação. RESULTADOS: Não foram verificadas diferenças significativas entre os instrumentos para o arroz, massas, carnes, refrigerantes e sucos artificiais. Os coeficientes de correlação corrigidos pela variabilidade intrapessoal variaram de -0,26 a 0,78. A concordância de classificação dos indivíduos no mesmo quartil de consumo para ambos os métodos variou de 22% (massas) a 50% (feijão). Para quartis opostos, os grupos que tiveram mais de 10% dos indivíduos classificados incorretamente foram massas (19%), carnes (13%) e gorduras (11%). Os valores de Kappa ponderado variaram de - 0,15 (massas) a 0,56 (feijão). O QFAA superestimou o consumo de quase a totalidade dos grupos alimentares e subestimou os grupos dos óleos, feijão, carnes e refrigerantes. CONCLUSÃO: O instrumento apresentou boa validade para feijão, verduras e legumes, leite e derivados, biscoitos recheados e para o arroz.

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This study aimed to describe the behavior of oviposition traps for Aedes aegypti over time, to compare it with the larval survey and to investigate the association with climatic variables. It was conducted in São José do Rio Preto city, São Paulo. Daily climatic data and fortnightly measurements for oviposition traps and larval infestation were collected from October 2003 to September 2004. Three different periods were identified in the behavior of oviposition traps' positivity and mean number of eggs: increase, plateau and decrease in values. These measurements followed the variation of climatic data from the first and third periods. High correlation was obtained between the positivity and the mean number of eggs. The oviposition traps showed higher capacity to detect the vector than did larval survey. It was observed that the first (October to December) and third (May to September) periods were considered to be the most suitable to use oviposition traps than larval surveys.

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A combination of trajectory sensitivity method and master-slave synchronization was proposed to parameter estimation of nonlinear systems. It was shown that master-slave coupling increases the robustness of the trajectory sensitivity algorithm with respect to the initial guess of parameters. Since synchronization is not a guarantee that the estimation process converges to the correct parameters, a conditional test that guarantees that the new combined methodology estimates the true values of parameters was proposed. This conditional test was successfully applied to Lorenz's and Chua's systems, and the proposed parameter estimation algorithm has shown to be very robust with respect to parameter initial guesses and measurement noise for these examples. Copyright (C) 2009 Elmer P. T. Cari et al.

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This work deals with an improved plane frame formulation whose exact dynamic stiffness matrix (DSM) presents, uniquely, null determinant for the natural frequencies. In comparison with the classical DSM, the formulation herein presented has some major advantages: local mode shapes are preserved in the formulation so that, for any positive frequency, the DSM will never be ill-conditioned; in the absence of poles, it is possible to employ the secant method in order to have a more computationally efficient eigenvalue extraction procedure. Applying the procedure to the more general case of Timoshenko beams, we introduce a new technique, named ""power deflation"", that makes the secant method suitable for the transcendental nonlinear eigenvalue problems based on the improved DSM. In order to avoid overflow occurrences that can hinder the secant method iterations, limiting frequencies are formulated, with scaling also applied to the eigenvalue problem. Comparisons with results available in the literature demonstrate the strength of the proposed method. Computational efficiency is compared with solutions obtained both by FEM and by the Wittrick-Williams algorithm.

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The effects of chromium or nickel oxide additions on the composition of Portland clinker were investigated by X-ray powder diffraction associated with pattern analysis by the Rietveld method. The co-processing of industrial waste in Portland cement plants is an alternative solution to the problem of final disposal of hazardous waste. Industrial waste containing chromium or nickel is hazardous and is difficult to dispose of. It was observed that in concentrations up to 1% in mass, the chromium or nickel oxide additions do not cause significant alterations in Portland clinker composition. (C) 2008 International Centre for Diffraction Data.

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Introduction. This protocol aims at detecting and quantifying quiescent infections of Colletotrichum musae on bananas. The principle, key advantages, starting plant material, time required and expected results are presented. Materials and methods. The materials required and details of the three steps of the protocol (fruit sampling, fruit ripening and anthracnose lesion quantification) are described. Possible troubleshooting is discussed. Results. The protocol results in the quantification of anthracnose lesions on the fruits, which makes it possible to predict postharvest losses due to anthracnose (peel rot), and also to propose a better management of postharvest fungicide applications.

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This work is a part of a taxonomic revision of the Neotropical genus Hortia (Rutaceae), where three names (H. colambiana Gleason. H. chocoensis Cuatrec., and H. badinii M. Lisboa ex Groppo) are proposed as synonyms of H. brasiliana Vand. ex DC., and the name H. badinii is here validated. Additionally, another name in the Rutaceae. Dictyoloma peruvianum Plana., is proposed as a synonym of D. vandellianum A. Juss. Notes on the type collection of D. vandellianum are provided.

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For obtaining accurate and reliable gene expression results it is essential that quantitative real-time RT-PCR (qRT-PCR) data are normalized with appropriate reference genes. The current exponential increase in postgenomic studies on the honey bee, Apis mellifera, makes the standardization of qRT-PCR results an important task for ongoing community efforts. For this aim we selected four candidate reference genes (actin, ribosomal protein 49, elongation factor 1-alpha, tbp-association factor) and used three software-based approaches (geNorm, BestKeeper and NormFinder) to evaluate the suitability of these genes as endogenous controls. Their expression was examined during honey bee development, in different tissues, and after juvenile hormone exposure. Furthermore, the importance of choosing an appropriate reference gene was investigated for two developmentally regulated target genes. The results led us to consider all four candidate genes as suitable genes for normalization in A. mellifera. However, each condition evaluated in this study revealed a specific set of genes as the most appropriated ones.