Sulfonyl-hydrazones of cyclic imides derivatives as potent inhibitors of the Mycobacterium tuberculosis protein tyrosine phosphatase B (PtpB)

Searching lead compounds for new antituberculosis drugs, the activity of synthetic sulfonamides and sulfonyl-hydrazones were assayed for their potential inhibitory activity towards a protein tyrosine phosphatase from Mycobacterium tuberculosis - PtpB. Four sulfonyl-hydrazones N-phenylmaleimide derivatives were active (compounds 14, 15, 19 and 21), and the inhibition of PtpB was found to be competitive with respect to the substrate p-nitrophenyl phosphate. Structure-based molecular docking simulations were performed and indicated that the new inhibitor candidates showed similar binding modes, filling the hydrophobic pocket of the protein by the establishment of van der Waals contacts, thereby contributing significantly to the complex stability.

2-(2-Nitroanilino)-5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophene-3-carbonitrile

The title compound, C(16)H(15)N(3)O(2)S, was synthesized by the reaction of 2-amino-5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophene-3-carbonitrile and o-fluoronitrobenzene. The thiophene and nitrophenyl rings and amino and carbonitrile groups are coplanar with a maximum deviation of 0.046 (2) angstrom and a dihedral angle of 0.92 (6)degrees between the rings. The cyclohepta ring adopts a chair conformation. Intramolecular N-H center dot center dot center dot O and C-H center dot center dot center dot S interactions occur. In the crystal, the molecules form layers that are linked by pi-pi stacking interactions between the thiophene and benzene rings [centroid-centroid distances = 3.7089 (12) and 3.6170 (12) angstrom].

Acute and chronic effects of exercise on inflammatory markers and B-type natriuretic peptide in patients with coronary artery disease

Few studies have prospectively addressed the effects of exercise in the inflammatory activity of patients with coronary artery disease (CAD). We sought to evaluate the consequences of an acute bout of exercise on inflammatory markers and BNP in untrained CAD patients before and after randomization to a training program. 34 CAD patients underwent a 50-min acute exercise session on a cycle-ergometer at 65% peak oxygen uptake before and after blood sampling. They were then randomized to a 4-month chronic exercise program (15 patients) or general lifestyle recommendations (19 patients), undergoing a new acute session of exercise after that. In the overall population, acute exercise caused a significant increase in C-reactive protein [CRP; 1.79 (4.49) vs. 1.94 (4.89) mg/L, P < 0.001], monokine induced by interferon-gamma [Mig; 351 (324) vs. 373 (330) pg/mL, P = 0.027] and vascular adhesion molecule-1 [VCAM-1; 226 (82) vs. 252 (110) pg/mL, P = 0.02]. After 4-months, in exercise-trained patients, there was a significant decrease in the inflammatory response provoked by the acute exercise compared to patients in the control group reflected by a significant decrease in the differences between rest and post-exercise levels of CRP [-0.29 (0.84) mg/L vs. -0.11 (0.21) mg/L, P = 0.05]. Resting BNP was also significantly lower in exercise-trained patients when compared to untrained controls [15.6 (16.2) vs. 9.7 (11.4) pg/mL, P = 0.04 and 19.2 (27.8) vs. 23.2 (27.5) pg/mL, P = 0.76; respectively]. Chronic exercise training might partially reverse the inflammatory response caused by acute exercise in CAD patients. These results suggest that regular exercise is an important nonpharmacological strategy to the improvement in inflammation in CAD patients.

Motor perseveration during an ""A not B"" task in children with intellectual disabilities

This study was designed to identify perseverative reaching tendencies in children with intellectual disabilities (ID), over a period of 1 year, by using a version of the Piagetian ""A not B"" task modified by Smith, Thelen, Titzer, and McLin (1999). Nine children (4.8 years old at the beginning of the study) with intellectual disabilities (ID) (eight with mild ID; one with moderate ID) were assessed every 3 months for approximately 1 year, totaling four assessments. The results indicate that in a majority of the cases perseveration was resilient, and that the visual system decoupled from the reaching, especially towards the later assessment periods at the end of the year. Across assessment periods variability seemed to increase in each trial (A1 through B2) for reached target. These individuals, vulnerable to distraction and attention and to short-term memory deficits, are easily locked into rigid modes of motor habits. They are susceptible to perseveration while performing simple task contexts that are typically designed for 10- to 12-month-old, normally-developing infants, therefore creating strong confinements to stable, rigid modes of elementary forms of behavior. (C) 2009 Elsevier B.V. All rights reserved.

Microstructural characterization of rapidly solidified and heat-treated Ti(92)B(8) eutectic alloy

In this work, Ti(92)B(8) alloy was processed via rapid solidification (splat-cooling) and then heat-treated at 700 degrees C and 1000 degrees C. A careful microstructural characterization indicated that, after rapid solidification, a very fine two-phase microstructure was produced with no significant saturation of B in alpha/beta Ti. There was no indication of amorphous formation in the rapidly solidified splats. Both alpha Ti and TiB were observed in the microstructures of the splats after heat-treatment at 700 degrees C and 1000 degrees C, confirming the stability of the alpha Ti+TiB two-phase region in this temperature range. (C) 2008 Elsevier Inc. All rights reserved.

Microstructural characterization of as-cast Cr-B alloys

Accurate knowledge of several Me-B (Me - Metal) phase diagrams are important to evaluate higher order systems such as Me-Si-B ternaries. This work presents results of microstructural characterization of as-cast Cr-B alloys which are significant to assess the liquid compositions associated to most of the invariant reactions of this system. Alloys of different compositions were prepared by arc melting pure Cr and B pressed powder mixtures under argon atmosphere in a water-cooled copper crucible with non-consumable tungsten electrode and titanium getter. The phases were identified by scanning electron microscopy (SEM), using back-scattered electron (BSE) image mode and X-ray diffraction (XRD). In general, a good agreement was found between our data and those from the currently accepted Cr-B phase diagram. (c) 2006 Elsevier Inc. All rights reserved.

Rapid solidification and phase stability evaluation of Ti-Si-B alloys

Ti-rich Ti-Si-B alloys can be considered for structural applications at high temperatures (max. 700 degrees C), however, phase equilibria data is reported only for T = 1250 degrees C. Thus, in this work the phase stability of this system has been evaluated at 700 degrees C. In order to attain equilibrium conditions in shorter time, rapid solidified samples have been prepared and carefully characterized. The microstructural characterization of the produced materials were based on X-ray diffraction (XRD), scanning electron microscopy (SEM-BSE), high resolution transmission electron microscopy (HRTEM), High Temperature X-ray diffraction with Synchrotron radiation (XRDSR) and Differential Scanning Calorimetry (DSC). Amorphous and amorphous with embedded nanocrystals have been observed after rapid solidification from specific alloy compositions. The values of the crystallization temperature (Tx) of the alloys were in the 509-647 degrees C temperature range. After Differential Scanning Calorimetry and High Temperature X-ray Diffraction with Synchrotron radiation, the alloys showed crystalline and basically formed by two or three of the following phases: alpha Ti, Ti(6)Si(2)B; Ti(5)Si(3); Ti(3)Si and TiB. It has been shown the stability of the Ti(3)Si and Ti(6)Si(2)B phases at 700 degrees C and the proposition of an isothermal section at this temperature. (C) 2011 Elsevier B.V. All rights reserved.

Magnetization studies of binary and ternary Co-rich phases of the Co-Si-B system

CoB, CO(2)B, CoSi, Co(2)Si and CO(5)Si(2)B phases can be formed during heat-treatment of amorphous co-Si-B soft magnetic materials. Thus, it is important to determine their magnetic behavior as a function of applied field and temperature. In this study, polycrystalline single-phase samples of the above phases were produced via arc melting and heat-treatment under argon. The single-phase nature of the samples was confirmed via X-ray diffraction experiments. AC and DC magnetization measurements showed that Co(2)Si and CO(5)Si(2)B phases are paramagnetic. Minor amounts of either Co(2)Si or CoSi(2) in the CoSi-phase sample suggested a paramagnetic behavior of the CoSi-phase, however, it should be diamagnetic as shown in the literature. The diamagnetic behavior of the CoB phase was also confirmed. The paramagnetic behavior of CO(5)Si(2)B is for the first time reported. The magnetization results of the phase CO(2)B have a ferromagnetic signature already verified on previous NMR studies. A detailed set of magnetization measurements of this phase showed a change of the easy magnetization axis starting at 70K, with a temperature interval of about 13K at a very small field of 1 mT. As the strength of the field is increased the temperature interval is enlarged. The strength of field at which the magnetization saturates increases almost linearly as the temperature is increased above 70K. The room temperature total magnetostriction of the CO(2)B phase was determined to be 8 ppm at a field of 1T. (C) 2010 Elsevier B.V. All rights reserved.

A study on the pretreatment of a sugarcane bagasse sample with dilute sulfuric acid

Experiments based on a 2(3) central composite full factorial design were carried out in 200-ml stainless-steel containers to study the pretreatment, with dilute sulfuric acid, of a sugarcane bagasse sample obtained from a local sugar-alcohol mill. The independent variables selected for study were temperature, varied from 112.5A degrees C to 157.5A degrees C, residence time, varied from 5.0 to 35.0 min, and sulfuric acid concentration, varied from 0.0% to 3.0% (w/v). Bagasse loading of 15% (w/w) was used in all experiments. Statistical analysis of the experimental results showed that all three independent variables significantly influenced the response variables, namely the bagasse solubilization, efficiency of xylose recovery in the hemicellulosic hydrolysate, efficiency of cellulose enzymatic saccharification, and percentages of cellulose, hemicellulose, and lignin in the pretreated solids. Temperature was the factor that influenced the response variables the most, followed by acid concentration and residence time, in that order. Although harsher pretreatment conditions promoted almost complete removal of the hemicellulosic fraction, the amount of xylose recovered in the hemicellulosic hydrolysate did not exceed 61.8% of the maximum theoretical value. Cellulose enzymatic saccharification was favored by more efficient removal of hemicellulose during the pretreatment. However, detoxification of the hemicellulosic hydrolysate was necessary for better bioconversion of the sugars to ethanol.

Scale-up of diluted sulfuric acid hydrolysis for producing sugarcane bagasse hemicellulosic hydrolysate (SBHH)

Sugarcane bagasse was pretreated with diluted sulfuric acid to obtain sugarcane bagasse hemicellulosic hydrolysate (SBHH). Experiments were conducted in laboratory and semi-pilot reactors to optimize the xylose recovery and to reduce the generation of sugar degradation products, as furfural and 5-hydroxy-methylfurfural (HMF). The hydrolysis scale-up procedure was based on the H-Factor, that combines temperature and residence time and employs the Arrhenius equation to model the sulfuric acid concentration (100 mg(acid)/g(dm)) and activation energy (109 kJ/mol). This procedure allowed the mathematical estimation of the results through simulation of the conditions prevailing in the reactors with different designs. The SBHH obtained from different reactors but under the same H-Factor of 5.45 +/- 0.15 reached similar xylose yield (approximately 74%) and low concentration of sugar degradation products, as furfural (0.082 g/L) and HMF (0.0071 g/L). Also, the highest lignin degradation products (phenolic compounds) were rho-coumarilic acid (0.15 g/L) followed by ferulic acid (0.12 g/L) and gallic acid (0.035 g/L). The highest concentration of ions referred to S (3433.6 mg/L), Fe (554.4 mg/L), K (103.9 mg/L), The H-Factor could be used without dramatically altering the xylose and HMF/furfural levels. Therefore, we could assume that H-Factor was directly useful in the scale-up of the hemicellulosic hydrolysate production. (C) 2009 Published by Elsevier Ltd.

Thermal expansion of the V(5)Si(3) and T(2) phases of the V-Si-B system investigated by high-temperature X-ray diffraction

The thermal expansion anisotropy of the V(5)Si(3) and T(2)-phase of the V-Si-B system were determined by high-temperature X-ray diffraction from 298 to 1273 K. Alloys with nominal compositions V(62.5)Si(37.5) (V5Si3 phase) and V(63)Si(12)B(25) (T(2)-phase) were prepared from high-purity materials through arc-melting followed by heat-treatment at 1873 K by 24 h, under argon atmosphere. The V(5)Si(3) phase exhibits thermal expansion anisotropy equals to 1.3, with thermal expansion coefficients along the a and c-axis equal to 9.3 x 10(-6) K(-1) and 11.7 x 10(-6) K(-1), respectively. Similarly, the thermal expansion anisotropy value of the T(2)-phase is 0.9 with thermal expansion coefficients equal to 8.8 x 10(-6) K(-1) and 8.3 x 10(-6) K(-1) along the, a and c-axis respectively. Compared to other isostructural silicides of the 5:3 type and the Ti(5)Si(3) phase, the V(5)Si(3) phase presents lower thermal expansion anisotropy. The T(2)-phase present in the V-Si-B system exhibits low thermal expansion anisotropy, as the T(2)-phase of the Mo-Si-B, Nb-Si-B and W-Si-B systems. (C) 2009 Elsevier Ltd. All rights reserved.

Biodegradable nanosize particles of poly(L,L-lactide)-b-poly(ethylene glycol)-b-poly(L,L-lactide)

Two series of poly(L,L-lactide-b-ethylene glycol-b-L,L-lactide) copolymers, PLA-PEO-PLA, were synthesized by polymerization Of L,L-lactide using a dihydroxy-terminated poly(ethylene glycol) (PEG) (M-n = 4000 or 600 g/mol) as coinitiator and stannous 2-ethylhexanoate, Sn(Oct)(2), as initiator. The synthesized copolymers have shown high stereoregularity as observed by C-13 NMR analyses. The nanoparticles were prepared by using a solvent diffusion method and the self-assemblage process and were characterized by NMR and SEM. It was possible to conclude that the self-assembled particles presented a core-shell structure characterized by a hydrophobic PLA core and a hydrophilic PEG shell, thus the NMR of the aqueous solutions indicated a quasi-solid behavior for the particles` interior. The diameters of the spherical particles as observed by SEM were in the 50-250 nm range, depending on the copolymer composition and the preparation procedure.

Effects of weld strength mismatch on J and CTOD estimation procedure for SE(B) specimens

This work examines the effect of weld strength mismatch on fracture toughness measurements defined by J and CTOD fracture parameters using single edge notch bend (SE(B)) specimens. A central objective of the present study is to enlarge on previous developments of J and CTOD estimation procedures for welded bend specimens based upon plastic eta factors (eta) and plastic rotational factors (r (p) ). Very detailed non-linear finite element analyses for plane-strain models of standard SE(B) fracture specimens with a notch located at the center of square groove welds and in the heat affected zone provide the evolution of load with increased crack mouth opening displacement required for the estimation procedure. One key result emerging from the analyses is that levels of weld strength mismatch within the range +/- 20% mismatch do not affect significantly J and CTOD estimation expressions applicable to homogeneous materials, particularly for deeply cracked fracture specimens with relatively large weld grooves. The present study provides additional understanding on the effect of weld strength mismatch on J and CTOD toughness measurements while, at the same time, adding a fairly extensive body of results to determine parameters J and CTOD for different materials using bend specimens with varying geometries and mismatch levels.

Effect of Ti and C additions on structural and magnetic properties of (Pr,Nd)-Fe-B nanocrystalline magnetic materials

Effects of titanium carbide (TiC) addition on structural and magnetic properties of isotropic (Pr,Nd)-Fe-B nanocrystalline magnetic materials have been investigated. In this work, we investigate the effect of TiC addition on a (Pr,Nd)-poor and B-rich composition, as well as on a B-poor and (Nd, Pr)-rich composition. Rapidly solidified (Pr, Nd)-Fe-B alloys were prepared by melt-spinning. The compositions studied were (Pr(1-x)Nd(x))(4)Fe(78)B(18) (x = 0, 0.5, and 1) with addition of 3 at% TiC. Unlike the (Pr(x)Nd(1-x))(9.5)Fe(84.5)B(6) materials that present excellent values for coercive. field and energy product, the (Pr,Nd)-poor and B-rich composition alloys with TiC addition present lower values. Rietveld analysis of X-ray data and Mossbauer spectroscopy revealed that samples are predominantly composed of Fe(3)B and alpha-Fe. For the RE-rich compositions (Pr(x)Nd(1-x))(9.5)Fe(84.5)B(6) (x = 0.1, 0.25, 0.5, 0.75, and 1) with the addition of 3 at% TiC, the highest coercive field and energy product (8.4 kOe and 14.4 MGOe, respectively) were obtained for the composition Pr(9.5)Fe(84.5)B(6). (c) 2008 Elsevier B.V. All rights reserved.

Effect of Calcium on the in vitro Growth of Aechmea blanchetiana (Baker) L. B. Smith Plantlets

This work investigated the influence of different concentrations of calcium on the growth of plantlets of the bromeliad Aechmea blanchetiana cultured in vitro. Seedlings of A. blanchetiana were axenically cultured in liquid Murashige and Skoog basal medium supplemented with different concentrations of calcium (Ca; 1.5, 3, 4.5, 6, or 12 mM) without growth regulators. The resulting plantlets were cultured under 93 mol m-2 s-1 illumination, 12 hour photoperiod regime and 25C 1 for 120 days with subculture to fresh identical media every 30 days. The addition of calcium at 9.38 mM to MS modified medium increased the production of fresh and dry mass of plantlets, whilst chlorine from calcium chloride dehydrate (CaCl2 2 H2O) in excess (3.35 mM) decreased both the fresh and dry mass of plantlets.