High precision and selectivity for quantitation of enrofloxacin and ciprofloxacin in five chicken tissues using solid phase extraction and ESI LC-MS/MS for application in monitoring residues

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

Selecting candidate labels for hierarchical document clusters using association rules

One way to organize knowledge and make its search and retrieval easier is to create a structural representation divided by hierarchically related topics. Once this structure is built, it is necessary to find labels for each of the obtained clusters. In many cases the labels have to be built using only the terms in the documents of the collection. This paper presents the SeCLAR (Selecting Candidate Labels using Association Rules) method, which explores the use of association rules for the selection of good candidates for labels of hierarchical document clusters. The candidates are processed by a classical method to generate the labels. The idea of the proposed method is to process each parent-child relationship of the nodes as an antecedent-consequent relationship of association rules. The experimental results show that the proposed method can improve the precision and recall of labels obtained by classical methods. © 2010 Springer-Verlag.

Improving hierarchical document cluster labels through candidate term selection

One way to organize knowledge and make its search and retrieval easier is to create a structural representation divided by hierarchically related topics. Once this structure is built, it is necessary to find labels for each of the obtained clusters. In many cases the labels must be built using all the terms in the documents of the collection. This paper presents the SeCLAR method, which explores the use of association rules in the selection of good candidates for labels of hierarchical document clusters. The purpose of this method is to select a subset of terms by exploring the relationship among the terms of each document. Thus, these candidates can be processed by a classical method to generate the labels. An experimental study demonstrates the potential of the proposed approach to improve the precision and recall of labels obtained by classical methods only considering the terms which are potentially more discriminative. © 2012 - IOS Press and the authors. All rights reserved.

Effects of gamma-irradiation on caprolactam level from multilayer PA-6 films for food packaging: Development and validation of a gas chromatographic method

A gas chromatographic method to determine caprolactam in multilayer PA-6 films used for meat foodstuffs and cheese was developed and validated. A wide linear range (0.8-400 mu g/ml), RSD <= 4.1% and recovery higher than 90.0% were obtained for the chromatographic system, while precision and accuracy of the method showed RSD <= 3.8%, recovery from 95.5-100.0% and LOQ of 32 mu g/g. Irradiated (3, 7 and 12 kGy) and non-irradiated commercial films were analyzed. Most of them increased caprolactam levels with the increase of irradiation doses. (C) 2008 Elsevier Ltd. All rights reserved.

Identification and migration of degradation compounds from irradiation of multilayer polyamide 6 films for meat foodstuffs and cheese

The aim of this work was to identify the degradation compounds produced during irradiation of multilayer polyamide 6 (PA-6) films and to study their migration into water and 95% ethanol food simulant. After irradiation of multilayer PA-6 films at 3, 7 and 12 kGy, degradation compounds were extracted using solid-phase microextraction, for which the time and temperature of extraction and stirring were optimized, and identified by gas chromatography-mass spectrometry. Caprolactam, 2-cyclopentylcyclopentanone and aldehydes, among other compounds, were identified in the headspace of the films. Polydimethylsiloxane was considered the best fiber for extraction. The optimum conditions of time, temperature and stirring to extract the compounds were 20 min, 80 degrees C and 225 rpm. For validation purposes, the compounds were quantified in water and 95% ethanol and the results showed high sensitivity, good precision and accuracy. Migration of compounds from irradiated and non-irradiated multilayer PA-6 films into water and 95% ethanol food simulants was carried out at 40 degrees C for 10 days. The method was efficient for the quantification of decaldehyde, 2-cyclopentylcyclopentanone and caprolactam that migrated from multilayer PA-6 films into food simulants.

Development and validation of a nonaqueous titration with perchloric acid to determine sparfloxacin in tablets

A simple, rapid and inexpensive method for the determination of sparfloxacin in tablets is described. The procedure is based on the use of volumetric dosage in a nonaqueous medium in glacial acetic acid with 0.1 M perchloric acid. The method validation yielded good results and included precision and accuracy. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Development and validation of HPLC method for analysis of dexamethasone acetate in microemulsions

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Development and application of methods for determination of residual monomer in dental acrylic resins using high performance liquid chromatography

Two high-performance liquid chromatographic methods for determination of residual monomer in dental acrylic resins are described. Monomers were detected by their UV absorbance at 230 nm, on a Nucleosil((R)) C-18 (5 mu m particle size, 100 angstrom pore size, 15 x 0.46 cm i.d.) column. The separation was performed using acetonitrile-water (55:45 v/v) containing 0.01% triethylamine (TEA) for methyl methacrylate and butyl methacrylate, and acetonitrile-water (60:40 v/v) containing 0.01% TEA for isobutyl methacrylate and 1,6-hexanediol dimethacrylate as mobile phases, at a flow rate of 0.8 mL/min. Good linear relationships were obtained in the concentration range 5.0-80.0 mu g/mL for methyl methacrylate, 10.0-160.0 mu g/mL for butyl methacrylate, 50.0-500.0 mu g/mL for isobutyl methacrylate and 2.5-180.0 mu g/mL for 1,6-hexanediol dimethacrylate. Adequate assay for intra- and inter-day precision and accuracy was observed during the validation process. An extraction procedure to remove residual monomer from the acrylic resins was also established. Residual monomer was obtained from broken specimens of acrylic disks using methanol as extraction solvent for 2 h in an ice-bath. The developed methods and the extraction procedure were applied to dental acrylic resins, tested with or without post-polymerization treatments, and proved to be accurate and precise for the determination of residual monomer content of the materials evaluated. Copyright (c) 2005 John Wiley & Sons, Ltd.

Spectrophotometric Determination of Captopril Through Charge Transfer Complex Formation Using Fractional Factorial and Central Composite Design

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Silver as internal standard for simultaneous determination of Cd and Pb in whole blood by electrothermal atomic absorption spectrometry

The use of internal standardization for simultaneous atomic absorption spectrometry (SIMAAS) was investigated for Cd and Pb determination in whole blood. The comparison of thermochemical and physicochemical parameters allowed the selection of Ag, Bi, and Tl as internal standard candidates. Correlation graphs, plotted from the normalized absorbance signals (n = 20) of internal standard (axis y) versus analyte ( axis x), precision and accuracy were used to select Ag as the most appropriate internal standard. Blood samples were diluted (1 + 9) with 0.11% (m/v) Triton X-100 + 1.1% (v/v) HNO3 + 0.28% (m/v) NH4H2PO4 + 10 mug L-1 Ag+. Pyrolysis and atomization temperatures for the optimized heating program were 550 and 1700 degreesC, respectively. Characteristic masses based on integrated absorbance were 1.68 +/- 0.01 pg for Cd and 30.3 +/- 0.1 pg for Pb. The detection limits (DL) were 0.095 +/- 0.001 mug L-1 and 0.86 +/- 0.01 mug L-1 for Cd and Pb, respectively. The mean RSD for all determinations was the same for Cd (13 +/- 9%) with or without Ag as internal standard ( IS). on the other hand, the use of Ag as IS improved the RSD for Pb from 3.6 +/- 4.0% to 2.2 +/- 2.0%. An effective contribution of the internal standard Ag was verified in the recoveries of spiked samples (0.5 mug L-1 Cd2+ and 5.0 mug L-1 Pb2+). The mean recoveries were 81 +/- 8% and 91 +/- 4% for Cd, and 80 +/- 11% and 93 +/- 6% for Pb without and with IS correction, respectively. This is the first application of IS for a simultaneous determination by SIMAAS.

Quantitative analysis of mineral content in enamel using synchrotron microtomography and microhardness analysis. - art. no. 631824

Synchrotron microtomography is a tool to quantify the mineralization of dental tissues as well as microhardness analysis, since they provide adequate precision and contrast sensitivity. This study evaluates synchrotron microtomography and microhardness analysis for quantifying the mineral content of bovine enamel. Fifty enamel blocks were submitted individually for 5 days to a pH-cycling model at 37 degrees C and remained in the remineralizing solution for 2 days. The blocks were treated twice daily for 1 min with NaF dentifrices (Placebo, 275, 550, 1,100 mu g F/g and Crest (R)) diluted in deionized water. Surface microhardness changes (%SMH) and mineral loss (Delta Z) were then calculated. Synchrotron microtomography was also used to measure total mineral lost (SMM). Pearson's correlation (p < 0.05) was used to determine the relationship between different methods of analysis and dose-response between treatments. Dentifrice fluoride concentration and %SMH and Delta Z were correlated (p < 0.05). There was a positive relationship (p < 0.05) when comparing SMM vs. Delta Z; a negative relationship (p < 0.05) was found for %SMH vs. SMM and %SMH vs. Delta Z. Based on the results of this study, it was possible to conclude that synchrotron microtomography provides the best spatial resolution and contrast sensitivity for quantifying mineral gradients.

Rapid, quantitative determination of polar compounds in fats and oils by solid-phase extraction and size-exclusion chromatography using monostearin as internal standard

A rapid and simple method was developed for quantitation of polar compounds in fats and oils using monostearin as internal standard. Starting from 50 mg of oil sample, polar compounds were obtained by solid-phase extraction (silica cartridges) and subsequently separated by high-performance size-exclusion chromatography into triglyceride polymers, triglyceride dimers, oxidized triglyceride monomers, diglycerides, internal standard and fatty acids. Quantitation of total polar compounds was achieved through the internal standard method and then amounts of each group of compounds could be calculated. A pool of polar compounds was used to check linearity, precision and accuracy of the method, as well as the solid-phase extraction recovery. The procedure was applied to samples with different content of polar compounds and good quantitative results were obtained, especially for samples of low alteration level.

Development and validation of an UV spectrophotometric method for determination of gatifloxacin in tablets

A simple, sensitive and accurate spectrophotometric method was developed for the assay of gatifloxacin in raw material and tablets. Validation of the method yielded good results concerning range, linearity, precision and accuracy. The absorbance was measured at 287 nm for gatifloxacin tablet solutions. The linearity range was found to be 4.0-14.0 μg/mL for gatifloxacin. It was also found that the excipients in the commercial tablets did not interfere with the method.

Development and validation of HPLC method for quantitative analysis of triamcinolone in biodegradable microparticles

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.

Determination of calcium and magnesium in hydroethanolic extracts of propolis by atomic absorption flame spectrophotometry

Propolis is a natural product collected by honeybees and has a large range of pharmacological activity, including antimicrobial, antitumoral, antioxidant and anti-inflammatory. Its use as a popular medicine is increasing all over the world, creating a need for quality control of the commercial products. In this study the levels of calcium and magnesium in commercial hydroalcoholic propolis extracts from varies states of Brazil were determined by atomic absorption flame spectrophotometry and different values were obtained for northern and southern states. This study can be extended to the analysis of metals that are harmful to health. The results showed that the calibration curves were linear over a wide concentration range (0.5-4.0 μg.mL -1 for calcium and 0.05-0.4 μg.mL -1 for magnesium) with good correlation coefficients (0.999 and 0.988, respectively). Good analytical recovery (94%) was obtained. The proposed method showed adequate precision and relative standard deviation lower than 2 %. The method is accurate and precise as well as having advantages such as simplicity and speed.