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.

Theory of non-steady state electrical characteristics of metal-insulator-metal structures with schottky barriers and exponentially distributed impurity states

We discuss non-steady state electrical characteristics of a metal-insulator-metal structure. We consider an exponential distribution (in energy) of impurity states in addition to impurity states at a single energy level within the depletion region. We discuss thermal as well as isothermal characteristics and present an expression for the temperature of maximum current (Tm) and a method to calculate the density of exponentially distributed impurity states. We plot the theoretical curves for various sets of parameters and the variation of Tm, and Im (maximum current) with applied potential for various impurity distributions. The present model can explain the available experimental results. Finally we compare the non-steady state characteristics in three cases: (i) impurity states only at a single energy level, (ii) uniform energetic distribution of impurity states, and (iii) exponential energetic distribution of impurity states.

Determination and persistence of methiocarb in artichokes

A simple and rapid method for the determination of methiocarb in artichokes by high-performance liquid chromatography with UV detection is described. No derivatization is needed and the limit of determination (0.01 ppm) is analogous to that of fluorometric detection. The results of trials carried out with granular and liquid formulations of this active ingredient are also reported. Immediately after treatment with the liquid formulation methiocarb residues averaged 1.47 ppm, while after treatment with the granular formulation residues were considered fortuitous. The decay rate of methiocarb residues in artichokes shows that the decrease and eventual disappearance of this active ingredient can chiefly be ascribed to the dilution effect due to head growth.

Optimization procedures in the design of continuous induction hardening and tempering installations for magnetic steel bars

An inverse problem concerning the industrial process of steel bars hardening and tempering is considered. The associated optimization problem is formulated in terms of membership functions and, for the sake of comparison, also in terms of quadratic residuals; both geometric and electromagnetic design variables have been considered. The numerical solution is achieved by coupling a finite difference procedure for the calculation of the electromagnetic and thermal fields to a deterministic strategy of minimization based on modified Flctcher and Reeves method. © 1998 IEEE.

Crystal structure of BaBi2Ta2O9

The crystal structure of the Aurivillius compound Bi2BaTa2O9 prepared via the chemical route was determined by direct methods using EXPO97, and refined using the Rietveld method with conventional X-ray diffraction data. The structure was found to be tetragonal (space group I4/mmm, number 139) and Z = 2, isomorphic of the Bi2BaNb2O9 reported by Blake and co-workers in the literature (1997). Two refinements were performed using the two asymmetry functions of DBWS-9807 (release 20/May/99). The unit cell for each case are: a = 3.932 22(6) Å, c = 25.5053(6) Å (RA) and a = 3.93250(7) Å, c = 25.5069(6) Å (RCF). The differences for atom positions, interatomic distances and angles are in the range of one standard deviation. Final agreements factors are: Rwp = 7.97%, S = 1.84, RBragg = 4.28%(RA), Rwp = 7.98%, S = 1.84, RBragg = 4.30% (RCF). The occupancies of Ba and Bi in site 2b were refined but constrained to have their summation equal to 1.00. The same constraints were applied to the Ba and Bi of the 4e site. The results show that on site 2b there are 70% of Ba and 30% of Bi and on the site 4e there are 82% of Bi and 18% of Ba. The charge equilibrium is maintained for one standard deviation of the site occupancies. © 2000 International Centre for Diffraction Data.

Constraints implementation for IQML and mode direction-of-arrival estimators

The iterative quadratic maximum likelihood IQML and the method of direction estimation MODE are well known high resolution direction-of-arrival DOA estimation methods. Their solutions lead to an optimization problem with constraints. The usual linear constraint presents a poor performance for certain DOA values. This work proposes a new linear constraint applicable to both DOA methods and compare their performance with two others: unit norm and usual linear constraint. It is shown that the proposed alternative performs better than others constraints. The resulting computational complexity is also investigated.

A simple and rapid extraction for gas chromatographic determination of thiabendazole and imazalil residues in lemons

A rapid and efficient method is described for the determination of thiabendazole and imazalil residues in lemons (peel and pulp). The procedure is based on the extraction with an hexane:ethyl acetate mixture (1:1, v/v) and gas chromatographic analysis using thermionic specific detection (TSD). The possibility of matrix effect was also studied. Mean recoveries from 8 replicates of fortified samples ranged from 79% to 109%, with relative standard deviation values between 2.4% to 12.8%. The detection and quantification limits of the method were 0.2 mg kg-1 and 0.5 mg kg-1, respectively.

Evaluation of marginal microleakage in Class II cavities: Effect of microhybrid, flowable, and compactable resins

Objective: The goal of the present study was to evaluate the microleakage on the cementum/dentin and enamel surfaces in Class II restorations, using different kinds of resin composite (microhybrid, flowable, and compactable). Method and materials: Forty human caries-free molars were extracted and selected. Eighty Class II standardized cavities were made in the cervical wall at the cementoenamel junction (CEJ) and at the mesial and distal surfaces. The teeth were divided into four groups: G1 - adhesive system + microhybrid resin composite Z100; G2 - adhesive system + compactable resin composite Prodigy Condensable; G3 - adhesive system + flowable resin composite Revolution + Z100 resin composite; G4 - adhesive system + Revolution fluid resin + compactable resin composite Prodigy Condensable. The adhesive system used in this study was Scotchbond Multi-Purpose Plus. The specimens were thermocycled in baths of 5°C and 55°C for 1,000 cycles and immersed in 50% silver nitrate solution. The specimens then were sectioned and evaluated on degree of dye penetration. Results: The results were evaluated using the nonparametric Kruskall-Wallis test, which showed a statistically significant difference between groups G1 and G4, G2 and G4, and G3 and G4. Conclusions: None of the materials was able to eliminate the marginal microleakage at the cervical wall; the application of a low-viscosity resin composite combined with a compactable resin composite significantly decreased the microleakage.

A method for the digital image analysis of ceramic grains based on shape factor segmentation

A very simple and robust method for ceramics grains quantitative image analysis is presented. Based on the use of optimal imaging conditions for reflective light microscopy of bulk samples, a digital image processing routine was developed for shading correction, noise suppressing and contours enhancement. Image analysis was done for grains selected according to their concavities, evaluated by perimeter ratio shape factor, to avoid consider the effects of breakouts and ghost boundaries due to ceramographic preparation limitations. As an example, the method was applied for two ceramics, to compare grain size and morphology distributions. In this case, most of artefacts introduced by ceramographic preparation could be discarded due to the use of perimeter ratio exclusion range.

Validation of UV spectrophotometric method for determination of lomefloxacin in pharmaceutical dosage form

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.

Farming technology, biochemistry characterization, and protective effects of culinary-medicinal mushrooms Agaricus brasiliensis S. Wasser et al. and Lentinus edodes (Berk.) Singer: Five years of research in Brazil

The biotechnology, biochemical characterization, and protective effects of the himematsutake and shiitake mushrooms were studied for the Thematic Project, from 1998 to 2003. A new species, Agaricus Brasiliens is Wasser et al. (= A. blazei Murrill ss. Heinem.), was proposed for the cultivated lineages in Brazil. Interactions among lineages, substrates, casing layers, and fructification inductions (temperature alternations) significantly increased the productivity of A. brasiliensis in Brazil (from 40 g to 200 g of fresh mushroom kg -1 moist compost). However, pests and diseases (mainly Sciaridae flies and false truffle), drastically reduced the productivity of A. brasiliensis (below 50 g kg -1). Biochemically for each mushroom species, the polar extracts, no polars, and medium polarity presented the same organic substances; however, their concentrations differed as a result of the lineages, maturation of the fruit bodies, and cultivation conditions. In this aspect, concentration of linoleic acid in A. brasiliensis (added to animal food) was related directly to the chemical protection against carcinogenic drugs in mice. Aqueous extracts of Lentinus edodes (= Lentinula edodes (Berk.) Pegler) and A. brasiliensis may be preventive chemical protectors against mutagenic and carcinogenic drugs, depending on the lineage and extraction method (tea or juice). However, immunomodulator effects and tumor reduction were only observed with concentrated fractions (hexanic, methanolic, and ATF extracts). Aqueous extracts of A. brasiliensis and L. edodes have antibiotic-like substances and substances able to act as elicitors of resistance responses in some plants (local and systemic) and show a potential to be used in the alternative control of plant pathogens. © 2005 by Begell House, Inc.

Propolis: anti-Staphylococcus aureus activity and synergism with antimicrobial drugs

Propolis is a natural resinous substance collected by bees from tree exudates and secretions. Its antimicrobial activity has been investigated and inhibitory action on Staphylococcus aureus growth was evaluated The in vitro synergism between ethanolic extract of propolis (EEP) and antimicrobial drugs by two susceptibility tests (Kirby and Bauer and E-Test) on 25 S. aureus strains was evaluated Petri dishes with sub-inhibitory concentrations of EEP were incubated with 13 drugs using Kirby and Bauer method and synergism between EEP and five drugs [choramphenicol (CLO), gentamicin (GEN), netilmicin (NET), tetracycline (TET), and vancomycin (VAN)] was observed. Nine drugs were assayed by the E-test method and five of them exhibited a synergism [CLO, GEN, NET, TET, and clindamycin (CLI)]. The results demonstrated the synergism between EEP and antimicrobial drugs, especially those agents that interfere on bacterial protein synthesis.

Lower intercanine width and gingival margin changes. A retrospective study.

OBJECTIVE: To determine if changes in the lower intercanine widths during orthodontic treatment with fixed appliances result in gingival margin changes around the lower canines and incisors. METHOD: Pre- and post-treatment intra-oral photographs and orthodontic study models of 178 Caucasian adolescents (101 female, 77 male) were used. All subjects were treated with fixed appliances. The subjects had mean ages of 11.41 (SD: 1.83) years and 14.91 (SD: 1.78) years on their initial and final records respectively. The latter were taken 28 days or more after the appliances had been removed. The inclusion criteria were: Angle Class I or Class II malocclusion (with or without transverse and/or vertical discrepancies); nonextraction treatment; less than 4 mm crowding or spacing; fully erupted lower incisors and good periodontal health. The intercanine widths and the positions of the gingival margins relative to the maximum curvatures of the labial surfaces of the lower canines and incisors were measured with digital calipers. RESULTS: A significant association was found between unaltered intercanine widths and coronal migration of the gingival margins (p = 0.045). There were no significant associations between either increased or reduced intercanine widths and changes in the gingival margins. CONCLUSIONS: Following orthodontic treatment coronal migration of the gingival margins around the lower incisors and canines is more likely to be associated with an unaltered intercanine width.

Bond strength durability of direct and indirect composite systems following surface conditioning for repair

Purpose: This study evaluated the effect of surface conditioning methods and thermocycling on the bond strength between a resin composite and an indirect composite system in order to test the repair bond strength. Materials and Methods: Eighteen blocks (5 x 5 x 4 mm) of indirect resin composite (Sinfony) were fabricated according to the manufacturer's instructions. The specimens were randomly assigned to one of the following two treatment conditions (9 blocks per treatment): (1) 10% hydrofluoric acid (HF) for 90 s (Dentsply) + silanization, (2) silica coating with 30-Ìm SiOx particles (CoJet) + silanization. After surface conditioning, the bonding agent was applied (Adper Single Bond) and light polymerized. The composite resin (W3D Master) was condensed and polymerized incrementally to form a block. Following storage in distilled water at 37°C for 24 h, the indirect composite/resin blocks were sectioned in two axes (x and y) with a diamond disk under coolant irrigation to obtain nontrimmed specimens (sticks) with approximately 0.6 mm2 of bonding area. Twelve specimens were obtained per block (N = 216, n = 108 sticks). The specimens from each repaired block were again randomly divided into 2 groups and tested either after storage in water for 24 h or thermocycling (6000 cycles, 5°C to 55°C). The microtensile bond strength test was performed in a universal testing machine (crosshead speed: 1 mm/min). The mean bond strengths of the specimens of each block were statistically analyzed using two-way ANOVA (α = 0.05). Results: Both surface conditioning (p = 0.0001) and storage conditions (p = 0.0001) had a significant effect on the results. After 24 h water storage, silica coating and silanization (method 2) showed significantly higher bond strength results (46.4 ± 13.8 MPa) than that of hydrofluoric acid etching and silanization (method 1) (35.8 ± 9.7 MPa) (p < 0.001). After thermocycling, no significant difference was found between the mean bond strengths obtained with method 1 (34.1 ± 8.9 MPa) and method 2 (31.9 ± 7.9 MPa) (p > 0.05). Conclusion: Although after 24 h of testing, silica coating and silanization performed significantly better in resin-resin repair bond strength, both HF acid gel and silica coating followed by silanization revealed comparable bond strength results after thermocycling for 6000 times.

Manganese determination by GFAAS in feces and fish feed slurries

This paper presents a simple, fast and sensitive method to determine manganese in samples of feces and fish feed by graphite furnace atomic absorption spectrometry (GFAAS) by the direct introduction of slurries into the graphite tube. The limits of detection (LOD) and quantification (LOQ) calculated for 20 readings of the blank of the standard slurries (0.50 % m/v of feces or feed devoid of manganese) were 28 and 92 μg kg-1 for the standard feces slurries and 34 and 110 μg kg-1 for the standard feed slurries. The proposed method was applied in bioavailability studies of manganese in different fish feeds and their results proved compatible with those obtained for samples mineralized by acid digestion using microwave oven. ©2007 Sociedade Brasileira de Química.