TEOR DE CAFEÍNA EM CAFÉS BRASILEIROS

Different brands and batches of brazilian regular and instant coffee were purchased in supermarkets of Campinas? city and analysed for caffeine content. The method used involved extraction with boiling water, clarification with saturated basic acetate and determination by high performance liquid cromatography. Analysis was carried out using a Model 6000 A solvent delivery system (Waters associates), and a Model 7125 sample injector system (Reodyne, Inc.) with a 5µl sample loop. The system was also equipped with a Waters Model M440 absorbance detector set at 254 nm. A Merck ODS 5µm column (15 cm x 4.6 mm i.d.) was used to separate the caffeine. The mobile phase was methanol:water (25:75, v/v). The caffeine content varied for different brands and types of coffee and according to the beverage preparation technique. Values in the range of 0.43 to 0.85 mg/ml and 0.61 to 0.82 mg/ml were determined in regular and instant coffee, respectively.

Hidrocarbonetos aromáticos policíclicos em margarina, creme vegetal e maionese

Polycyclic aromatic hydrocarbons (PAHs) are a group of compounds that have been the subject of much concern due to their toxic potential. In this study, margarine?s, vegetable cream and mayonnaise available on the Brazilian market were analyzed for pyrene, chrysene, benzo(a)pyrene, benzo(b)fluoranthene and dibenzo(a,h)anthracene. The analytical methodology involved liquid-liquid extraction, clean-up on silica gel column and determination by high performance liquid chromatography using fluorescence detector. Variable levels of contamination were found within differents brands of the same product and within differents batches of the same brand. The total PAH content was in the range of 4.1 to 7.1mug/kg in vegetable cream, 1.7 to 3.9mug/kg in margarine and 1.0 to 21.7mug/kg in mayonnaise. In general the products which according to the label contain corn oil showed the highest levels of contamination. Based on these results and on the importance of fat, oils and derived products for the intake of PAHs, it is recommended that producers of margarine, vegetable creams and mayonnaise start to control the contamination of the vegetable oils used in the elaboration of these products, in order to reduce the exposure of consumers to excessive amounts of potentially carcinogenic compounds.

Desenvolvimento de ferramentas de análise de desempenho de atletas em 3 diferentes modalidades : Handebol, Provas Combinadas e Salto com Vara

Universidade Estadual de Campinas. Faculdade de Educação Física

Validity and reliability of methods for the detection of secondary caries around amalgam restorations in primary teeth

Secondary caries has been reported as the main reason for restoration replacement. The aim of this in vitro study was to evaluate the performance of different methods - visual inspection, laser fluorescence (DIAGNOdent), radiography and tactile examination - for secondary caries detection in primary molars restored with amalgam. Fifty-four primary molars were photographed and 73 suspect sites adjacent to amalgam restorations were selected. Two examiners evaluated independently these sites using all methods. Agreement between examiners was assessed by the Kappa test. To validate the methods, a caries-detector dye was used after restoration removal. The best cut-off points for the sample were found by a Receiver Operator Characteristic (ROC) analysis, and the area under the ROC curve (Az), and the sensitivity, specificity and accuracy of the methods were calculated for enamel (D2) and dentine (D3) thresholds. These parameters were found for each method and then compared by the McNemar test. The tactile examination and visual inspection presented the highest inter-examiner agreement for the D2 and D3 thresholds, respectively. The visual inspection also showed better performance than the other methods for both thresholds (Az = 0.861 and Az = 0.841, respectively). In conclusion, the visual inspection presented the best performance for detecting enamel and dentin secondary caries in primary teeth restored with amalgam.

Chemical composition, acetylcholinesterase inhibitory and antifungal activities of Pera glabrata (Schott) Baill. (Euphorbiaceae)

Pera glabrata (Schott) Baill. was selected for this study after showing a preliminary positive result in a screening of Atlantic Forest plant species in the search for acetylcholinesterase inhibitors and antifungal compounds. The bioassays were conducted with crude ethanol extract of the leaves using direct bioautography method for acetylcholinesterase and antifungal activities. This extract was partitioned with hexane, chloroform and ethyl acetate solvents. The active chloroform fraction was submitted to silica gel chromatography column affording 12 groups. Caffeine, an alkaloid, which showed detection limits of 0.1 and 1.0 µg for anticholinesterasic and antifungal activities, respectively, was isolated from group nine. After microplate analyses, only groups four, nine, 10, 11 and 12 showed acetylcholinesterase inhibitory activity of 40% or higher. The group 12 was purified by preparative layer chromatography affording four sub-fractions. Two sub-fractions from this group were analyzed by gas chromatography-mass spectrometry and gas chromatography-flame ionization detector. The first sub-fraction showed anticholinesterasic activity and contained two major compounds: 9-hydroxy-4-megastigmen-3-one (84%) and caffeine (6%). The second sub-fraction presented five major compounds identified as 9-hydroxy-4-megastigmen-3-one, isololiolide, (-) loliolide, palmitic acid and lupeol and did not show activity.

VUV spectral line emission measurements in the TCABR tokamak

The study of tokamak plasma light emissions in the vacuum ultraviolet (VUV) region is an important subject since many impurity spectral emissions are present in this region. These spectral emissions can be used to determine the plasma ion temperature and density from different species and spatial positions inside plasma according to their temperatures. We have analyzed VUV spectra from 500 Å to 3200 Å wavelength in the TCABR tokamak plasma including higher diffraction order emissions. There have been identified 37 first diffraction order emissions, resulting in 28 second diffraction order, 24 third diffraction order, and 7 fourth diffraction order lines. The emissions are from impurity species such as OII, OIII, OIV, OV, OVI, OVII, CII, CIII, CIV, NIII, NIV, and NV. All the spectra beyond 1900 Å are from higher diffraction order emissions, and possess much better spectral resolution. Each strong and isolated spectral line, as well as its higher diffraction order emissions suitable for plasma diagnostic is identified and discussed. Finally, an example of ion temperature determination using different diffraction order is presented.

Study of mural paintings by Fulvio Pennacchi in São Paulo City by mineralogical techniques

The present research deals with two mural paintings made in 1947 with the fresco technique by Fulvio Pennacchi in the Catholic Chapel of the Hospital das Clínicas (São Paulo City, Brazil), namely the Virgin Annunciation and the Supper at Emmaus. This study regards the materials and painting techniques used by the artist, based on historical research,on in situ observations and laboratory analytical techniques (stereomicroscopy,scanning electron microscopy with an energy dispersive spectrometer, X-ray diffractometry, electron microprobe, images obtained with UV-light), aiming to improve the methods of characterization of objects of our cultural heritage, and to enhance its preservation accordingly. The results lead to the identification of the plaster components and of distinct layers in the frescoes, besides further information on grain size, impurities and textures, composition of pigments, and features of deterioration, such as efflorescences. The degree of degradation of the murals painting was assessed by this way. Our data suggest that a single layer of plaster was used by Pennacchi, as a common mortar with fine- and medium-grained aggregates. Differences in texture were obtained by adding gypsum to the plaster.

On-line identification of minor flavones from sugarcane juice by LC/UV/MS and post-column derivatization

This work describes the on-line characterization of minor flavones from sugarcane (Saccharum officinarum) juice by high-performance liquid chromatography coupled to diode array UV detection and mass spectrometry (LC/UV/MS) using atmospheric pressure chemical ionization-collision-induced dissociation (APCI-CID-MS/MS) and post-column derivatization using UV shift reagents. HPLC-UV analysis with shift reagents provided information about the substitution pattern in the flavonoid skeleton and, combined with MS data, these techniques allowed for the on-line identification of five "garapa" flavones: luteolin-8-C-glucosyl-7-O-glucuronide; tricin-7-O-neohesperoside-4'-O-rhamnoside; tricin-7-O-methylglucuronate-4'-O-rhamnoside; tricin-7-O-methylglucuronide; swertisin, while four other compounds were partially identified as glycosylflavones. Only swertisin (7-O-methylapigenin-6-C-glucoside) was reported previously in sugarcane molasses.

Design, construction and evaluation of a simple pressurized solvent extraction system

This work describes the construction and testing of a simple pressurized solvent extraction (PSE) system. A mixture of acetone:water (80:20), 80 ºC and 103.5 bar, was used to extract two herbicides (Diuron and Bromacil) from a sample of polluted soil, followed by identification and quantification by high-performance liquid chromatography coupled with diode array detector (HPLC-DAD). The system was also used to extract soybean oil (70 ºC and 69 bar) using pentane. The extracted oil was weighed and characterized through the fatty acid methyl ester analysis (myristic (< 0.3%), palmitic (16.3%), stearic (2.8%), oleic (24.5%), linoleic (46.3%), linolenic (9.6%), araquidic (0.3%), gadoleic (< 0.3%), and behenic (0.3%) acids) using high-resolution gas chromatography with flame ionization detection (HRGC-FID). PSE results were compared with those obtained using classical procedures: Soxhlet extraction for the soybean oil and solid-liquid extraction followed by solid-phase extraction (SLE-SPE) for the herbicides. The results showed: 21.25 ± 0.36% (m/m) of oil in the soybeans using the PSE system and 21.55 ± 0.65% (m/m) using the soxhlet extraction system; extraction efficiency (recovery) of herbicides Diuron and Bromacil of 88.7 ± 4.5% and 106.6 ± 8.1%, respectively, using the PSE system, and 96.8 ± 1.0% and 94.2 ± 3.9%, respectively, with the SLP-SPE system; limit of detection (LOD) and limit of quantification (LOQ) for Diuron of 0.012 mg kg-1 and 0.040 mg kg-1, respectively; LOD and LOQ for Bromacil of 0.025 mg kg-1 and 0.083 mg kg-1, respectively. The linearity used ranged from 0.04 to 1.50 mg L-1 for Diuron and from 0.08 to 1.50 mg L-1 for Bromacil. In conclusion, using the PSE system, due to high pressure and temperature, it is possible to make efficient, fast extractions with reduced solvent consumption in an inert atmosphere, which prevents sample and analyte decomposition.

Demonstrando os fundamentos, potencialidades e limitações da análise por injeção seqüencial

The sensitivity and accuracy of sequential injection methods are dependent on efficient overlapping of reagent and sample zones as they are propelled toward the detector cell. The formation of the reduced phosphomolybdic acid is used to demonstrate that the overlapping efficiency in a fixed reaction coil relies on a suitable choice of reagent to sample volume ratio. Additionally, under poor mixing conditions or highly concentrated samples, the reaction extension is strongly dependent on the reagent concentration. The zone-sampling concept is exploited to determine phosphate in cola-based soft drinks after in-line dilution in an auxiliary coil.

A biosensor based on immobilization of lactate oxidase in a PB-CTAB film for FIA determination of lactate in beer samples

An amperometric lactate biosensor with lactate oxidase immobilized into a Prussian Blue (PB) modified electrode was fabricated. The advantage of using cetyltrimethylammonium bromide (CTAB) in the electrodeposition step of PB films onto glassy carbon surfaces was confirmed taking into account both the stability and sensitivity of the measurements. The biosensor was used in the development of a FIA amperometric method for the determination of lactate. Under optimal operating conditions (pH = 6.9, E = -0.1 V), the linear response of the method was extended up to 0.28 µmol L-1 lactate with a limit of detection of 0.84 mmol L-1. The repeatability of the method for injections of a 0.28 mmol L-1 lactate solution was 2.2 % (n = 18). The usefulness of the method was demonstrated by determining lactate in beer samples and the results were in good agreement with those obtained by using a reference spectrophotometric enzyme method.

New constraints on muon-neutrino to electron-neutrino transitions in MINOS

This paper reports results from a search for nu(mu) -> nu(e) transitions by the MINOS experiment based on a 7 x 10(20) protons-on-target exposure. Our observation of 54 candidate nu(e) events in the far detector with a background of 49.1 +/- 7.0(stat) +/- 2.7(syst) events predicted by the measurements in the near detector requires 2sin(2)(2 theta(13))sin(2)theta(23) < 0.12(0.20) at the 90% C.L. for the normal (inverted) mass hierarchy at delta(CP) = 0. The experiment sets the tightest limits to date on the value of theta(13) for nearly all values of delta(CP) for the normal neutrino mass hierarchy and maximal sin(2)(2 theta(23)).

Search for sterile neutrino mixing in the MINOS long-baseline experiment

A search for depletion of the combined flux of active neutrino species over a 735 km baseline is reported using neutral-current interaction data recorded by the MINOS detectors in the NuMI neutrino beam. Such a depletion is not expected according to conventional interpretations of neutrino oscillation data involving the three known neutrino flavors. A depletion would be a signature of oscillations or decay to postulated noninteracting sterile neutrinos, scenarios not ruled out by existing data. From an exposure of 3.18 x 10(20) protons on target in which neutrinos of energies between similar to 500 MeV and 120 GeV are produced predominantly as nu(mu), the visible energy spectrum of candidate neutral-current reactions in the MINOS far detector is reconstructed. Comparison of this spectrum to that inferred from a similarly selected near-detector sample shows that of the portion of the nu(mu) flux observed to disappear in charged-current interaction data, the fraction that could be converting to a sterile state is less than 52% at 90% confidence level (C. L.). The hypothesis that active neutrinos mix with a single sterile neutrino via oscillations is tested by fitting the data to various models. In the particular four-neutrino models considered, the mixing angles theta(24) and theta(34) are constrained to be less than 11 degrees and 56 degrees at 90% C. L., respectively. The possibility that active neutrinos may decay to sterile neutrinos is also investigated. Pure neutrino decay without oscillations is ruled out at 5.4 standard deviations. For the scenario in which active neutrinos decay into sterile states concurrently with neutrino oscillations, a lower limit is established for the neutrino decay lifetime tau(3)/m(3) > 2.1 x 10(-12) s/eV at 90% C.L.

Search for Muon-Neutrino to Electron-Neutrino Transitions in MINOS

This Letter reports on a search for nu(mu)->nu(e) transitions by the MINOS experiment based on a 3.14x10(20) protons-on-target exposure in the Fermilab NuMI beam. We observe 35 events in the Far Detector with a background of 27 +/- 5(stat)+/- 2(syst) events predicted by the measurements in the Near Detector. If interpreted in terms of nu(mu)->nu(e) oscillations, this 1.5 sigma excess of events is consistent with sin(2)(2 theta(13)) comparable to the CHOOZ limit when |Delta m(2)|=2.43x10(-3) eV(2) and sin(2)(2 theta(23))=1.0 are assumed.

Observation of double electron-positron pair production by gamma rays reexamined

An experiment was conducted to observe triple- and quadruple-escape peaks, at a photon energy equal to 6.128 MeV, in the spectra recorded with a high-purity Ge detector working in coincidence with six bismuth germanate detectors. The peak intensities may be explained having recourse to only the bremsstrahlung cascade process of consecutive electron-positron pair creation; i.e., the contribution of simultaneous double pair formation (and other cascade effects) is much smaller. The experimental peak areas are in reasonably good agreement with those predicted by Monte Carlo simulations done with the general-purpose radiation-tran sport code PENELOPE.