911 resultados para 2D chromatography


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A simple and fast multiresidue method has been developed to determine 48 pesticides within the major groups of pesticides (organohalogen, organophosphorous, pyrethroids and organonitrogen) in representative samples of locally produced honey, in Bauru (State of São Paulo, Brazil) during 2003-2004. The recovery results found ranged from 76% to 95% and the limits of detection were lower than 0.01 mg/kg for gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC-MS-SIM). The results indicated that most pesticides found in the samples belonged to the organohalogen and organophosphorous groups and lower levels of residues of some organonitrogen and pyretroids were also detected. Malathion residues were detected in all the samples, in a high concentration, owing to its applications to control dengue mosquitoes in the area studied. (c) 2005 Elsevier Ltd. All rights reserved.

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In Fazenda Belém oil field (Potiguar Basin, Ceará State, Brazil) occur frequently sinkholes and sudden terrain collapses associated to an unconsolidated sedimentary cap covering the Jandaíra karst. This research was carried out in order to understand the mechanisms of generation of these collapses. The main tool used was Ground Penetrating Radar (GPR). This work is developed twofold: one aspect concerns methodology improvements in GPR data processing whilst another aspect concerns the geological study of the Jandaíra karst. This second aspect was strongly supported both by the analysis of outcropping karst structures (in another regions of Potiguar Basin) and by the interpretation of radargrams from the subsurface karst in Fazenda Belém. It was designed and tested an adequate flux to process GPR data which was adapted from an usual flux to process seismic data. The changes were introduced to take into account important differences between GPR and Reflection Seismic methods, in particular: poor coupling between source and ground, mixed phase of the wavelet, low signal-to-noise ratio, monochannel acquisition, and high influence of wave propagation effects, notably dispersion. High frequency components of the GPR pulse suffer more pronounced effects of attenuation than low frequency components resulting in resolution losses in radargrams. In Fazenda Belém, there is a stronger need of an suitable flux to process GPR data because both the presence of a very high level of aerial events and the complexity of the imaged subsurface karst structures. The key point of the processing flux was an improvement in the correction of the attenuation effects on the GPR pulse based on their influence on the amplitude and phase spectra of GPR signals. In low and moderate losses dielectric media the propagated signal suffers significant changes only in its amplitude spectrum; that is, the phase spectrum of the propagated signal remains practically unaltered for the usual travel time ranges. Based on this fact, it is shown using real data that the judicious application of the well known tools of time gain and spectral balancing can efficiently correct the attenuation effects. The proposed approach can be applied in heterogeneous media and it does not require the precise knowledge of the attenuation parameters of the media. As an additional benefit, the judicious application of spectral balancing promotes a partial deconvolution of the data without changing its phase. In other words, the spectral balancing acts in a similar way to a zero phase deconvolution. In GPR data the resolution increase obtained with spectral balancing is greater than those obtained with spike and predictive deconvolutions. The evolution of the Jandaíra karst in Potiguar Basin is associated to at least three events of subaerial exposition of the carbonatic plataform during the Turonian, Santonian, and Campanian. In Fazenda Belém region, during the mid Miocene, the Jandaíra karst was covered by continental siliciclastic sediments. These sediments partially filled the void space associated to the dissolution structures and fractures. Therefore, the development of the karst in this region was attenuated in comparison to other places in Potiguar Basin where this karst is exposed. In Fazenda Belém, the generation of sinkholes and terrain collapses are controlled mainly by: (i) the presence of an unconsolidated sedimentary cap which is thick enough to cover completely the karst but with sediment volume lower than the available space associated to the dissolution structures in the karst; (ii) the existence of important structural of SW-NE and NW-SE alignments which promote a localized increase in the hydraulic connectivity allowing the channeling of underground water, thus facilitating the carbonatic dissolution; and (iii) the existence of a hydraulic barrier to the groundwater flow, associated to the Açu-4 Unity. The terrain collapse mechanisms in Fazenda Belém occur according to the following temporal evolution. The meteoric water infiltrates through the unconsolidated sedimentary cap and promotes its remobilization to the void space associated with the dissolution structures in Jandaíra Formation. This remobilization is initiated at the base of the sedimentary cap where the flow increases its abrasion due to a change from laminar to turbulent flow regime when the underground water flow reaches the open karst structures. The remobilized sediments progressively fill from bottom to top the void karst space. So, the void space is continuously migrated upwards ultimately reaching the surface and causing the sudden observed terrain collapses. This phenomenon is particularly active during the raining season, when the water table that normally is located in the karst may be temporarily located in the unconsolidated sedimentary cap

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Difusive processes are extremely common in Nature. Many complex systems, such as microbial colonies, colloidal aggregates, difusion of fluids, and migration of populations, involve a large number of similar units that form fractal structures. A new model of difusive agregation was proposed recently by Filoche and Sapoval [68]. Based on their work, we develop a model called Difusion with Aggregation and Spontaneous Reorganization . This model consists of a set of particles with excluded volume interactions, which perform random walks on a square lattice. Initially, the lattice is occupied with a density p = N/L2 of particles occupying distinct, randomly chosen positions. One of the particles is selected at random as the active particle. This particle executes a random walk until it visits a site occupied by another particle, j. When this happens, the active particle is rejected back to its previous position (neighboring particle j), and a new active particle is selected at random from the set of N particles. Following an initial transient, the system attains a stationary regime. In this work we study the stationary regime, focusing on scaling properties of the particle distribution, as characterized by the pair correlation function ø(r). The latter is calculated by averaging over a long sequence of configurations generated in the stationary regime, using systems of size 50, 75, 100, 150, . . . , 700. The pair correlation function exhibits distinct behaviors in three diferent density ranges, which we term subcritical, critical, and supercritical. We show that in the subcritical regime, the particle distribution is characterized by a fractal dimension. We also analyze the decay of temporal correlations

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The aim of this study was to compare the stress distribution induced by posterior functional loads on conventional complete dentures and implant-retained overdentures with different attachment systems using a two-dimentional Finite Element Analysis (FEA-2D). Three models representative of edentulous mandible were constructed on AutoCAD software; Group A (control), a model of edentulous mandible supporting a complete denture; Group B, a model of edentulous mandible supporting an overdenture over two splinted implants connected with the bar-clip system; Group C, a model of edentuluos mandible supporting an overdenture over two unsplinted impants with the O-ring system. Evaluation was conducted on Ansys software, with a vertical force of 100 N applied on the mandibular left first molar. When the stress was evaluated in supporting tissues, groups B (51.0 MPa) and C (52.6 MPa) demonstrated higher stress values than group A (10.1 MPa). Within the limits of this study, it may be conclued that the use of an attachment system increased stress values; furthermore, the use of splinted implants associated with the bar-clip attachment system favoured a lower stress distribution over the supporting tissue than the unsplinted implants with an O-ring abutment to retain the manibular overdenture.

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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.

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The high performance liquid chromatography (HPLC) technique was applied to measure phenylalanine ammonia-lyase (PAL, EC 4.3.1.5) activity in soybean (Glycine max L. Merril cv. BR16) roots. t-Cinnamate, the catalytic product of the PAL reaction was quantified at 275 nm by isocratic elution with methanol:water through an ODS(M) column. Comparative experiments were carried out with 1.0 mM ferulic acid, an inducer of PAL activity. The results suggest that liquid chromatography is a rapid and sensitive method to analyze PAL activity in non-purified extract.

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The methanolic extract of the bark of the medicinal plant Qualea parviflora (Vochysiaceae) contains new nor-seco-triterpene and pentacyclic triterpenoids. They were separated in a preparative scale using droplet counter-current chromatography. The optimum solvent used was composed of a mixture of CHCl3/MeOH/H2O (43:37:20, v/v) in the descending mode and led to a successful separation of the new compound 28-nor-17, 22-seco-2 alpha, 3 beta, 19, 22, 23-pentahydroxy-Delta(12)-olecinane, besides the known triterpenoids bellericagenin B, bellericaside B and arjunglucoside I. Identification was performed by ESI-MS, H-1 NMR and C-13 NMR analyses.

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The methanolic extract of the leaves of the medicinal plant Byrsonima crassa (Malpighiaceae) contain flavonoids with antioxidant activity. They were separated in a preparative scale using high-speed counter-current chromatography. The optimum solvent system used was composed of a mixture of ethyl acetate-n-propanol-water (140:8:80 (v/v/v)) and led to a successful separation between monoglucosilated flavonoids (quercetin-3-O-alpha-L-arabinoside, quercetin-3-O-beta-D-galactoside) and the biflavonoid amentoflavone in only 3.5 h. The purities of quercetin-3-O-alpha-L-arabinoside (95 mg), quercetin-3-O-beta-D-galactoside (16 mg) and the biflavonoid amentoflavone (114 mg) were all isolated at purity over 95%. Identification was performed by H-1 NMR, C-13 NMR and UV analyses. (C) 2004 Published by Elsevier B.V.

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