865 resultados para Validation of analytical methods


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E-Science experiments typically involve many distributed services maintained by different organisations. After an experiment has been executed, it is useful for a scientist to verify that the execution was performed correctly or is compatible with some existing experimental criteria or standards, not necessarily anticipated prior to execution. Scientists may also want to review and verify experiments performed by their colleagues. There are no existing frameworks for validating such experiments in today's e-Science systems. Users therefore have to rely on error checking performed by the services, or adopt other ad hoc methods. This paper introduces a platform-independent framework for validating workflow executions. The validation relies on reasoning over the documented provenance of experiment results and semantic descriptions of services advertised in a registry. This validation process ensures experiments are performed correctly, and thus results generated are meaningful. The framework is tested in a bioinformatics application that performs protein compressibility analysis.

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Propolis obtained from honeybee hives has been widely used in medicine, cosmetics, and industry due to its versatile biological activities (antioxidant, antimicrobial, fungicidal, antiviral, antiulcer, immunostimulating, and cytostatic). These activities are mainly attributed to the presence of flavonoids in propolis, which points out the interest in quantifying these constituents in propolis preparations, as well as validation of analytical methodologies. High-performance liquid chromatography (HPLC) methods have been reported to quantify isolated flavonoids or these compounds in complex biological matrices, such as herbal raw materials and extractive preparations. An efficient, precise, and reliable method was developed for quantification of propolis extractive solution using HPLC with UV detection. The chromatograms were obtained from various gradient elution systems (GES) tested in order to establish the ideal conditions for the analysis of propolis extractive solution, using methanol and water: acetonitrile (97.5 : 2.5, v/v) as mobile phase. Gradient reversed phase chromatography was performed using a stainless steel column (250 x 4.6 mm i.d., 5 mum) filled with Chromsep RP 18 (Varian), column temperature at 30.0 +/- 0.1degreesC and detection at 310 nm. The main validation parameters of the method were also determined. The method showed linearity for chrysin in the range 0.24-2.4 mug mL(-1) with good correlation coefficients (0.9975). Precision and accuracy were determined. The obtained results demonstrate the efficiency of the proposed method. The analytical procedure is reliable and offers advantages in terms of speed and cost of reagents.

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Cyclic oligomers were identified in PET bottles used for mineral water and fruit juice using MS and H-1 and C-13 NMR: a first series cyclic trimer, a first series cyclic tetramer, a first series cyclic dimmer and a second series cyclic trimer. An analytical method to determine first series cyclic trimer in these bottles was developed and validated, using HPLC. The first series cyclic trimer levels were 316-462 mg/100 g of PET bottle. (c) 2005 Elsevier B.V. All rights reserved.

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

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Abnormal intragastric distribution of food (IDF) and a phasic contractility in the proximal stomach have been related to dyspeptic symptoms. Thus, the behaviour of the stomach and the proximal region, in particular, continues to attract attention and demand for reliable and comfortable techniques. The aims of this study were to employ AC Biosus-ceptometry (ACB) and scintigraphy to evaluate IDF and gastric motor activity in humans. Fifteen healthy volunteers ingested 60 mL of yogurt containing 2 mCi of Tc-99m and 4 g of ferrite. Each volunteer had gastric motility and IDF evaluated twice on separate days; on one occasion by ACB and another by scintigraphy. Digital signal processing was performed in MatLab (Mathworks Inc., Natick, MA, USA). Results were expressed as mean +/- SD. Similar results of distal accumulation time (P < 0.001) were obtained for scintigraphy (6.93 +/- 3.25 min) and for ACB (7.04 +/- 3.65 min). Fast Fourier Transform revealed two dominant frequencies (P > 0.9). Besides the well-know frequency of 3 cpm, our results showed identical frequencies in proximal stomach recordings (P < 0.001) for scintigraphic (1.01 +/- 0.01 cpm) and ACB (0.98 +/- 0.06 cpm). In summary, our data showed that scintigraphy and ACB are promising techniques to evaluate several aspects of gastric motility. Moreover, ACB is non-invasive, radiation-free and deserves the same importance as conventional methods for this kind of analysis.

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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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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Objective. To use the Pediatric Rheumatology International Trials Organization (PRINTO) core set of outcome measures to develop a validated definition of improvement for the evaluation of response to therapy in juvenile systemic lupus erythematosus (SLE).Methods. Thirty-seven experienced pediatric rheumatologists from 27 countries, each of whom had specific experience in the assessment of juvenile SLE patients, achieved consensus on 128 patient profiles as being clinically improved or not improved. Using the physicians' consensus ratings as the gold standard measure, the chi-square, sensitivity, specificity, false-positive and false-negative rates, area under the receiver operating characteristic curve, and kappa level of agreement for 597 candidate definitions of improvement were calculated. Only definitions with a kappa value greater than 0.7 were retained. The top definitions were selected based on the product of the content validity score multiplied by its kappa statistic.Results. The definition of improvement with the highest final score was at least 50% improvement from baseline in any 2 of the 5 core set measures, with no more than 1 of the remaining worsening by more than 30%.Conclusion. PRINTO proposes a valid and reproducible definition of improvement that reflects well the consensus rating of experienced clinicians and that incorporates clinically meaningful change in core set measures in a composite end point for the evaluation of global response to therapy in patients with juvenile SLE. The definition is now proposed for use in juvenile SLE clinical trials and may help physicians to decide whether a child with SLE responded adequately to therapy.

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Because the lack of textbooks based on electromyographic studies in the area of exercises for physical conditioning, the authors proposed to study the trapezius (upper portion) (TS) and the serratus anterior (lower portion) (SI) muscles during the execution of four different modalities of rowing exercises with middle grip in 24 male volunteers, 18 to 25 years old. For the recordings, it was used a two-channel TECA TE 4 electromyograph and Hewlett Packard surface electrodes. For the movements, a supine bench and a 120 cm-long bar made of low weight wood were used. The results showed that TS acted significantly in upright, sitting and inclined rowing, justifying its inclusion in physical conditioning programmes, while SI, in spite of acting preferentially in upright and sitting rowing, presented activity levels which do not justify its inclusion.

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A simple and reproducible method was developed for the assay of lomefloxacin in tablets. The excipients in the commercial tablet preparation did not interfere with the assay. Beer's law is obeyed in the range 2.0-9.0 μg.mL-1 at λmax 280 nm. The molar absorptivity was calculated. Six triplicate analyses of solutions containing six different concentrations of the examined drug were carried out and gave a mean correlation coefficient 0.9997. The proposed method was applied to the determination of the examined drug in coated tablet and the results demonstrated that the method is equally accurate, precise and reproducible as the official methods.

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A simple, rapid, selective and specific high performance liquid chromatographic (HPLC) method for quantitative analysis of the triamcinolone in polylactide-co-glycolide acid (PLGA) microparticles was developed. The chromatographic parameters were reversed-phase C18 column, 250mm x 4.6mm, with particle size 5 μm. The column oven was thermostated at 35°C ± 2°C. The mobile phase was methanol/water 45:55 (v/v) and elution was isocratic at a flow-rate of 1 mL.mL-1. The determinations were performed using a UV-Vis detector at 239 nm. The injected sample volume was 10 μL. The standard curve was linear (r2 > 0.999) in the concentration range 100-2500 ng.mL-1. The method showed adequate precision, with a relative standard deviation (RSD) was smaller than 3%. The accuracy was analyzed by adding a standard drug and good recovery values were obtained for all drug concentrations used. The method showed specificity and selectivity with linearity in the working range and good precision and accuracy, making it very suitable for quantitation of triamcinolone in PLGA microparticles.

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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.