12 resultados para solid state

em Biblioteca Digital da Produção Intelectual da Universidade de São Paulo


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The filamentous fungus Paecylomices variotii was able to produce high levels of cell extract and extracellular invertases when grown under submerged fermentation (SbmF) and solid-state fermentation, using agroindustrial products or residues as substrates, mainly soy bran and wheat bran, at 40A degrees C for 72 h and 96 h, respectively. Addition of glucose or fructose (a parts per thousand yen1%; w/v) in SbmF inhibited enzyme production, while the addition of 1% (w/v) peptone as organic nitrogen source enhanced the production by 3.7-fold. However, 1% (w/v) (NH4)(2)HPO4 inhibited enzyme production around 80%. The extracellular form was purified until electrophoretic homogeneity (10.5-fold with 33% recovery) by DEAE-Fractogel and Sephacryl S-200 chromatography. The enzyme is a monomer with molecular mass of 102 kDa estimated by SDS-PAGE with carbohydrate content of 53.6%. Optima of temperature and pH for both, extracellular and cell extract invertases, were 60A degrees C and 4.0-4.5, respectively. Both invertases were stable for 1 h at 60A degrees C with half-lives of 10 min at 70A degrees C. Mg2+, Ba2+ and Mn2+ activated both extracellular and cell extract invertases from P. variotii. The kinetic parameters K-m and V-max for the purified extracellular enzyme corresponded to 2.5 mM and 481 U/mg prot(-1), respectively.

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A series of heavy metal oxide (HMO) glasses with composition 26.66B(2)O(3)-16GeO(2)-4 Bi2O3-(53.33-x)PbO-xPbF2 (0 <= x <= 40) were prepared and characterized with respect to their bulk (glass transition and crystallization temperatures, densities, molar volumes) and spectroscopic properties. Homogeneous glasses are formed up to x = 30, while crystallization of beta-PbF2 takes place at higher contents. Substitution of PbO by PbF2 shifts the optical band gap toward higher energies, thereby extending the UV transmission window significantly toward higher frequencies. Raman and infrared absorption spectra can be interpreted in conjunction with published reference data. Using B-11 and F-19 high-resolution solid state NMR as well as B-11/F-19 double resonance methodologies, we develop a quantitative structural description of this material. The fraction of four-coordinate boron is found to be moderately higher compared to that in glasses with the same PbO/B2O3 ratios, suggesting some participation of PbF2 in the network transformation process. This suggestion is confirmed by the F-19 NMR spectra. While the majority of the fluoride ions is present as ionic fluoride, similar to 20% of the fluorine inventory acts as a network modifier, resulting in the formation of four-coordinate BO3/2F- units. These units can be identified by F-19{B-11} rotational echo double resonance and B-11{F-19} cross-polarization magic angle spinning (CPMAS) data. These results provide the first unambiguous evidence of B-F bonding in a PbF2-modified glass system. The majority of the fluoride ions are found in a lead-dominated environment. F-19-F-19 homonuclear dipolar second moments measured by spin echo decay spectroscopy are quantitatively consistent with a model in which these ions are randomly distributed within the network modifier subdomain consisting of PbO, Bi2O3, and PbF2. This model, which implies both the features of atomic scale mixing with the network former borate species and some degree of fluoride ion clustering is consistent with all of the experimental data obtained on these glasses.

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Current studies about lipase production involve the use of agro-industrial residues and newly isolated microorganisms aimed at increasing economic attractiveness of the process. Based on these aspects, the main objective of this work is to perform the partial characterization of enzymatic extracts produced by a newly isolated Penicillium crustosum in solid-state fermentation. Lipase extract presented optimal temperature and pH of 37 A degrees C and 9-10, respectively. The concentrated enzymatic extract showed more stability at 25 A degrees C and pH 7. The enzymes kept 100% of their enzymatic activity until 60 days of storage at 4 and -10 A degrees C. The stability under calcium salts indicated that the hydrolytic activity presented decay with the increase of calcium concentration. The specificity under several substrates indicated good enzyme activities in triglycerides from C4 to C18.

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Humicola brevis var. thermoidea cultivated under solid state fermentation in wheat bran and water (1:2 w/v) was a good producer of beta-glucosidase and xylanase. After optimization using response surface methodology the level of xylanase reached 5,791.2 +/- A 411.2 U g(-1), while beta-glucosidase production was increased about 2.6-fold, reaching 20.7 +/- A 1.5 U g(-1). Cellulase levels were negligible. Biochemical characterization of H. brevis beta-glucosidase and xylanase activities showed that they were stable in a wide pH range. Optimum pH for beta-glucosidase and xylanase activities were 5.0 and 5.5, respectively, but the xylanase showed 80 % of maximal activity when assayed at pH 8.0. Both enzymes presented high thermal stability. The beta-glucosidase maintained about 95 % of its activity after 26 h in water at 55 A degrees C, with half-lives of 15.7 h at 60 A degrees C and 5.1 h at 65 A degrees C. The presence of xylose during heat treatment at 65 A degrees C protected beta-glucosidase against thermal inactivation. Xylanase maintained about 80 % of its activity after 200 h in water at 60 A degrees C. Xylose stimulated beta-glucosidase activity up to 1.7-fold, at 200 mmol L-1. The notable features of both xylanase and beta-glucosidase suggest that H. brevis crude culture extract may be useful to compose efficient enzymatic cocktails for lignocellulosic materials treatment or paper pulp biobleaching.

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We present a detailed study of the Baryscan technique, a new efficient alternative to the widespread Z-scan technique which has been demonstrated [Opt. Lett. 36:8, 2011] to reach among the highest sensitivity levels. This method is based upon the measurement of optical nonlinearities by means of beam centroid displacements with a position sensitive detector and is able to deal with any kind of lensing effect. This technique is applied here to measure pump-induced electronic refractive index changes (population lens), which can be discriminated from parasitic thermal effects by using a time-resolved Baryscan experiment. This method is validated by evaluating the polarizability variation at the origin of the population lens observed in the reference Cr3+:GSGG laser material.

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In this study, Cross-Polarization Magic-angle Spinning CP/MAS, 2D Exchange, Centerband-Only Detection of Exchange (CODEX), and Separated-Local-Field (SLF) NMR experiments were used to study the molecular dynamics of poly(ethylene glycol) (PEG) inside Hectorite/PEG intercalation compounds in both single- and double-layer configurations. The results revealed that the overall amplitude of the motions of the PEG chain in the single-layer configuration is considerably smaller than that observed for the double-layer intercalation compound. This result indicates that the effect of having the polymer chain interacting with both clay platelets is to produce a substantial decrease in the motional amplitudes of those chains. The presence of these dynamically restricted segments might be explained by the presence of anchoring points between the clay platelets and the PEG oxygen atoms, which was induced by the Na+ cations. By comparing the PEG motional amplitudes of the double-layered nanocomposites composed of polymers with different molecular weights, a decrease in the motional amplitude for the smaller PEG chain was observed, which might also be understood using the presence of anchoring points.

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The intermetallic compounds ScPdZn and ScPtZn were prepared from the elements by high-frequency melting in sealed tantalum ampoules. Both structures were refined from single crystal X-ray diffractometer data: YAlGe type, Cmcm, a = 429.53(8), b = 907.7(1), c = 527.86(1) pm, wR2 = 0.0375, 231 F2 values, for ScPdZn and a = 425.3(1), b = 918.4(2), c = 523.3(1) pm, wR2 = 0.0399, 213 F2 values for ScPtZn with 14 variables per refinement. The structures are orthorhombically distorted variants of the AlB2 type. The scandium and palladium (platinum atoms) build up ordered networks Sc3Pd3 and Sc3Pt3 (boron networks) which are slightly shifted with respect to each other. These networks are penetrated by chains of zinc atoms (262 pm in ScPtZn) which correspond to the aluminum positions, i.e. Zn(ScPd) and Zn(ScPt). The corresponding group-subgroup scheme and the differences in chemical bonding with respect to other AlB2-derived REPdZn and REPtZn compounds are discussed. 45Sc solid state NMR spectra confirm the single crystallographic scandium sites. From electronic band structure calculations the two compounds are found metallic with free electron like behavior at the Fermi level. A larger cohesive energy for ScPtZn suggests a more strongly bonded intermetallic than ScPdZn. Electron localization and overlap population analyses identify the largest bonding for scandium with the transition metal (Pd, Pt).

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The dependences of phase stability and solid state phase transitions on the crystallite size in ZrO2-10, 12 and 14 mol% Sc2O3 nanopowders are investigated by X-ray powder diffraction using a synchrotron source (S-XPD). The average crystallite sizes lie within the range of 35 to 100 nm, approximately. At room temperature these solid solutions were previously characterised as mixtures of a cubic phase and one or two rhombohedral phases, beta and gamma, with their fractions depending on composition and average crystallite sizes. In this study, it is shown that at high temperatures these solid solutions become cubic single-phased. The size-dependent temperatures of the transitions from the rhombohedral phases to the cubic phase at high temperature are determined through the analyses of a number of S-XPD patterns. These transitions were studied on cooling and on heating, exhibiting hysteresis effects whose relevant features are size and composition dependent.

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This work aimed at evaluating the spray congealing method for the production of microparticles of carbamazepine combined with a polyoxylglyceride carrier. In addition, the influence of the spray congealing conditions on the improvement of drug solubility was investigated using a three-factor, three-level Box-Behnken design. The factors studied were the cooling air flow rate, atomizing pressure, and molten dispersion feed rate. Dependent variables were the yield, solubility, encapsulation efficiency, particle size, water activity, and flow properties. Statistical analysis showed that only the yield was affected by the factors studied. The characteristics of the microparticles were evaluated using X-ray powder diffraction, scanning electron microscopy, differential scanning calorimetry, and hot-stage microscopy. The results showed a spherical morphology and changes in the crystalline state of the drug. The microparticles were obtained with good yields and encapsulation efficiencies, which ranged from 50 to 80% and 99.5 to 112%, respectively. The average size of the microparticles ranged from 17.7 to 39.4 mu m, the water activities were always below 0.5, and flowability was good to moderate. Both the solubility and dissolution rate of carbamazepine from the spray congealed microparticles were remarkably improved. The carbamazepine solubility showed a threefold increase and dissolution profile showed a twofold increase after 60 min compared to the raw drug. The Box-Behnken fractional factorial design proved to be a powerful tool to identify the best conditions for the manufacture of solid dispersion microparticles by spray congealing.

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In this work, the temperature impact on the off-state current components is analyzed through numerical simulation and experimentally. First of all, the band-to-band tunneling is studied by varying the underlap in the channel/drain junction, leading to an analysis of the different off-state current components. For pTFET devices, the best behavior for off-state current was obtained for higher values of underlap (reduced BTBT) and at low temperatures (reduced SRH and TAT). At high temperature, an unexpected off-state current occurred due to the thermal leakage current through the drain/channel junction. Besides, these devices presented a good performance when considering the drain current as a function of the drain voltage, making them suitable for analog applications. (C) 2012 Elsevier Ltd. All rights reserved.

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CONTEXT: Esophageal dysphagia is the sensation that the ingested material has a slow transit or blockage in its normal passage to the stomach. It is not always associated with motility or transit alterations. OBJECTIVES: To evaluate in normal volunteers the possibility of perception of bolus transit through the esophagus after swallows of liquid and solid boluses, the differences in esophageal contraction and transit with these boluses, and the association of transit perception with alteration of esophageal contraction and/or transit. METHODS: The investigation included 11 asymptomatic volunteers, 4 men and 7 women aged 19-58 years. The subjects were evaluated in the sitting position. They performed swallows of the same volume of liquid (isotonic drink) and solid (macaroni) boluses in a random order and in duplicate. After each swallow they were asked about the sensation of bolus passage through the esophagus. Contractions and transit were evaluated simultaneously by solid state manometry and impedance. RESULTS: Perception of bolus transit occurred only with the solid bolus. The amplitude and area under the curve of contractions were higher with swallows of the solid bolus than with swallows of the liquid bolus. The difference was more evident in swallows with no perception of transit (n = 12) than in swallows with perception (n = 10). The total bolus transit time was longer for the solid bolus than for the liquid bolus only with swallows followed by no perception of transit. CONCLUSION: The results suggest that the perception of esophageal transit may be the consequence of inadequate adaptation of esophageal transit and contraction to the characteristics of the swallowed bolus.

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5E-Phenylethenylbenzofuroxan (5PhEBfx) was reported as an excellent anti-Chagas drug candidate. However, its oral bioavailability was affected by the crystallization process. Two samples exhibiting variable in vivo activity was investigated: a thin yellow powder (5PhEBfx-Y) and orange needles (5PhEBfx-O). X-ray powder diffraction, differential scanning calorimetry, vibrational spectroscopy, optical and electron scanning microscopies were applied to investigate both solid forms in order to correlate the solid-state properties with the variable bioavailability of 5PhEBfx. It was observed that 5PhEBfx-Y have a better solubility and consequently higher bioavailability when compared with 5PhEBfx-O. This result suggests that the difference of activity between these two 5E-Phenylethenylbenzofuroxanes could be associated with the solid forms, which also cause the coloration variation.