Degree of conversion of nanofilled and microhybrid composite resins photo-activated by different generations of LEDs

Objective: This study aimed at evaluating the degree of conversion (DC) of four composite resins, being one nanofilled and 3 microhybrid resins, photo-activated with second- and third-generation light-emitting diodes (LEDs). Material and methods: Filtek (TM) Z350 nanofilled composite resins and Amelogen (R) Plus, Vit-l-escence (TM) and Opallis microhybrid resins were photo-activated with two second-generation LEDs (Radii-cal and Elipar Free Light (TM) 2) and one third-generation LED (Ultra-Lume LED 5) by continuous light mode, and a quartz halogen-tungsten bulb (QHT, control). After 24 h of storage, the samples were pulverized into fine powder and 5 mg of each material were mixed with 100 mg of potassium bromide (KBr). After homogenization, they were pressed, which resulted in a pellet that was evaluated using an infrared spectromer (Nexus 470, Thermo Nicolet) equipped with TGS detector using diffuse reflectance (32 scans, resolution of 4 cm(-1)) coupled to a computer. The percentage of unreacted carbon-carbon double bonds (% C=C) was determined from the ratio of absorbance intensities of aliphatic C=C (peak at 1637 cm-1) against internal standard before and after curing of the specimen: aromatic C-C (peak at 1610 cm-1). Results: The ANOVA showed a significant effect on the interaction between the light-curing units (LCUs) and the composite resins (p<0.001). The Tukey's test showed that the nanofilled resin (Filtek (TM) Z350) and Opallis when photo-activated by the halogen lamp (QTH) had the lowest DC compared with the other microhybrid composite resins. The DC of the nanofilled resin (Filtek (TM) Z350) was also lower using LEDs. The highest degrees of conversion were obtained using the third-generation LED and one of second-generation LEDs (Elipar Free Light (TM) 2). Conclusions: The nanofilled resin showed the lowest DC, and the Vit-l-escence (TM) microhybrid composite resin showed the highest DC. Among the LCUs, it was not possible to establish an order, even though the second-generation LED Radii-cal provided the lowest DC.

Padronização interna em espectrometria de absorção atômica

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

Optimization of photo-polymerized sol gel monolithic stationary phases prepared in polyacrylate-coated fused-silica capillaries for capillary electrochromatography

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determination of olive oil acidity by CE

In this work, a CE method for the determination of olive oil acidity was proposed. The method was based on an ethanolic extraction (at 60 degrees C) of the oil long-chain free fatty acids (LC-FFAs) components followed by CE determination in pH 6.86 phosphate buffer at 15 mmol/L concentration containing 4 mmol/L sodium dodecylbenzenesulfonate (SDBS), 10 mmol/L polyoxyethylene 23 lauryl ether (Brij 35((R))), 2% v/v 1-octanol and 45% v/v ACN under indirect UV detection at 224 nm. Although this electrolyte promoted baseline separation of myristic acid (C14:0) (internal standard (IS)) and olive oil major components (palmitic acid (C16:0), oleic acid (C18:1c) and linoleic acid (C18:2cc)) in less than 8 min, after a few injections, the electropherogram profiles were severely altered (peak broadening, migration time shifts, etc.) and the current increased substantially. An adsorption study was conducted revealing that the dissolution of the capillary external polyimide coating during the electrophoretic run caused the detrimental effect. After removal of the capillary tip coating, ten consecutive injections could be performed without any disturbances and this simple procedure was, therefore, implemented during quantitative purposes. The reliability of the proposed method was further investigated by the determination of acidity of an extra virgin olive oil sample in comparison to the established methodology (AOCS method Ca 5a40, alkaline volumetric titration (AVT)). No statistical differences were found within 95% confidence level. A % acidity of 0.39 +/- 0.02 was found for the olive oil sample under consideration.

A Simple Method Based on ICP-MS for Estimation of Background Levels of Arsenic, Cadmium, Copper, Manganese, Nickel, Lead, and Selenium in Blood of the Brazilian Population

Throughout the world, biomonitoring has become the standard for assessing exposure of individuals to toxic elements as well as for responding to serious environmental public health problems. However, extensive biomonitoring surveys require rapid and simple analytical methods. Thus, a simple and high-throughput method is proposed for the determination of arsenic (As), cadmium (Cd), copper (Cu), manganese (Mn), nickel (Ni), lead (Pb), and selenium (Se) in blood samples by using inductively coupled plasma-mass spectrometry (ICP-MS). Prior to analysis, 200 l of blood samples was mixed with 500 l of 10% v/v tetramethylammonium hydroxide (TMAH) solution, incubated for 10 min, and subsequently diluted to 10 ml with a solution containing 0.05% w/v ethylenediamine tetraacetic acid (EDTA) + 0.005% v/v Triton X-100. After that, samples were directly analyzed by ICP-MS (ELAN DRC II). Rhodium was selected as an internal standard with matrix-matching calibration. Method detection limits were 0.08, 0.04, 0.5, 0.09, 0.12, 0.04, and 0.1 g//L for As, Cd, Cu, Mn, Ni, Pb, and Se, respectively. Validation data are provided based on the analysis of blood samples from the trace elements inter-\comparison program operated by the Institut National de Sante Publique du Quebec, Canada. Additional validation was provided by the analysis of human blood samples by the proposed method and by using electrothermal atomic absorption spectrometry (ETAAS). The method was subsequently applied for the estimation of background metal blood values in the Brazilian population. In general, the mean concentrations of As, Cd, Cu, Mn, Ni, Pb, and Se in blood were 1.1, 0.4, 890, 9.6, 2.1, 65.4, and 89.3 g/L, respectively, and are in agreement with other global populations. Influences of age, gender, smoking habits, alcohol consumption, and geographical variation on the values were also considered. Smoking habits influenced the levels of Cd in blood. The levels of Cu, Mn, and Pb were significantly correlated with gender, whereas Cu and Pb were significantly correlated with age. There were also interesting differences in Mn and Se levels in the population living in the north of Brazil compared to the south.

Determination of cobalt marker in cow ruminal fluid by EDXRF and SRTXRF

This article describes a comparison of conventional energy-dispersive X-ray fluorescence (EDXRF) and synchrotron radiation total-reflection X-ray fluorescence (SRTXRF) for Co determination in ruminal fluid from Holstein cow. This element is used as marker for animal nutrition studies. For EDXRF, 200 mu l of the sample were dried on 6.35 mu m Mylar filmat 60 degrees C. The excitation was carried out using an X-ray tube with Mo target and Zr filter operated at 30 kV/ 20 mA. For SRTXRF, 10 mu l of the samplewere pipetted on a Lucite carrier and dried at 60 degrees C. In both the techniques, Ga was used as internal standard and the acquisition time was 200 s. The trueness of both techniques was evaluated through the standard addition method, the recoveries obtained by SRTXRF and EDXRF were 76 and 99%, and the limits of detection, 13 and 240 mu g l(-1), respectively. Copyright (C) 2011 John Wiley & Sons, Ltd.

ASSESSMENT of POLYATOMIC INTERFERENCES ELIMINATION USING A COLLISION REACTION INTERFACE (CRI) FOR INORGANIC ANALYSIS of FUEL ETHANOL BY ICP-QMS

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

Determination of the geometrical diarylpropenamine isomers in feces by high-performance liquid chromatography

Diarylpropenamine derivatives are a class of compounds which have been evaluated as potential drug candidates. Here a specific and reproducible HPLC method for the determination of cis- and trans-isomers of the unsubstituted derivative, 3-(4'-bromo-[1,1'-biphenyl]-4-yl)-3-(4-X-phenyl-N,N-dimethyl-2-propen-1-amine (I, where X=H) in feces is described. The analyte I and internal standard, nitro derivative (II, where X=NO2), were isolated from the basified biological matrix using a liquid-liquid extraction with ethyl acetate followed by a solid-phase procedure performed on a silica cartridge. The organic phase was evaporated to dryness, the residue was reconstituted in mobile phase and injected into the HPLC system. The analytes were eluted with ethyl acetate-hexane-triethylamine (59:40:1) in HPLC column (silica) and detected by UV spectrophotometry at 272 nm. Linearity, precision and accuracy data for feces standards after extraction were acceptable. The method has been applied to analyses of feces samples from rats dosed with I, in which it could be anticipated that fecal excretion is quantitatively the major route for I elimination. Copyright (C) 1999 Elsevier Science B.V.

Quantification of sex pheromone from Anocentor nitens by gas chromatography-mass spectrometry-selected ion monitoring

Two highly sensitive and selective methods based on gas chromatography coupled to mass spectrometry (GC-MS) in the selected ion monitoring (SIM) mode have been developed for the quantification of 2,6-dichlorophenol (2,6-DCP), a sex pheromone of the tick females of Anocentor nitens. Standard addition method and calibration curve techniques using 5-bromine-4-hydroxy-3- methoxybenzaldehyde (5-BrV) as internal standard (IS) afforded detection limit of 0.1ngml-1. The calibration curve was linear over the concentration range from 0.5 to 500ngml-1 for 2,6-DCP. Results show that the concentration range of sex pheromone in the extracts samples was 1.08-10.35ngml-1. The methods developed provided reliable procedures to determine amounts of 2,6-DCP present in ticks. © 2003 Elsevier B.V. All rights reserved.

Evaluation of degree of conversion and hardness of dental composites photoactivated with different light guide tips

Objective: The aim of this study was to evaluate the degree of conversion and hardness of different composite resins, photo-activated for 40 s with two different light guide tips, fiber optic and polymer. Methods: Five specimens were made for each group evaluated. The percentage of unreacted carbon double bonds (% C=C) was determined from the ratio of absorbance intensities of aliphatic C=C (peak at 1637 cm-1) against internal standard before and after curing of the specimen: aromatic C-C (peak at 1610 cm-1. The Vickers hardness measurements were performed in a universal testing machine. A 50 gf load was used and the indenter with a dwell time of 30 seconds. The degree of conversion and hardness mean values were analyzed separately by ANOVA and Tukey's test, with a significance level set at 5%. Results: The mean values of degree of conversion for the polymer and fiber optic light guide tip were statistically different (P<.001). The hardness mean values were statistically different among the light guide tips (P<.001), but also there was difference between top and bottom surfaces (P<.001). Conclusions: The results showed that the resins photo-activated with the fiber optic light guide tip promoted higher values for degree of conversion and hardness.

An HPLC-UV method for the quantification of zidovudine in rat plasma

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

Farmacocinética pré-clínica do hidroximetilnitrofural (NFOH) – potencial pró-fármaco antichagásico

Pós-graduação em Ciências Farmacêuticas - FCFAR

Farmacocinética pré-clínica do composto 1-(2,6-diclorofenil)indolin-2-ona (DICCIC), pró-fármaco de diclofenaco

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

Contamination of cachaca by pahs from storage containers

Cachaça is a distiled beverage obtained from the fermentation of sugar cane syrup that, depending on the production procedures, may be susceptible to contamination by polycyclic aromatic hydrocarbons (PAHs). These compounds present carcinogenic and/or mutagenic properties and offer a risk to human health. Sixteen PAHs were determined in cachaças that had been stored in glass bottles and in polyethylene tank by gas chromatography coupled with mass spectrometry. The quantification of the PAHs utilised an internal standard. The limits of detection and quantification varied from 0.05 to 0.10 μg L−1 and 0.20 to 0.30 μg L−1, respectively. A total PAH concentration of 51.57 μg L−1 was found in the beverages that were stored in the tank, while the concentration in the cachaça stored in glass jugs was 6.07 μg L−1. These results indicate that the polyethylene tank is a source for PAHs in cachaça.

Avaliação de interface de reação e colisão para eliminar interferências poliatômicas na análise de etanol combustível por ICP-MS

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)