Antimycobacterial and antitumor activities of Palladium(II) complexes containing isonicotinamide (isn): X-ray structure of trans-[Pd(N(3))(2)(isn)(2)]

Complexes of the type trans-[PdX(2)(isn)(2)] {X = Cl (1), N(3) (2), SCN (3), NCO (4); isn = isonicotinamide} were synthesized and evaluated for in vitro antimycobacterial and antitumor activities. The coordination mode of the isonicotinamide and the pseudohalide ligands was inferred by IR spectroscopy. Single crystal X-ray diffraction determination on 2 showed that coordination geometry around Pd(II) is nearly square planar, with the ligands in a trans configuration. All the compounds demonstrated better in vitro activity against Mycobacterium tuberculosis than isonicotinamide and pyrazinamide. Among the complexes, compound 2 was found to be the most active with MIC of 35.89 mu M. Complexes 1-4 were also screened for their in vitro antitumor activity towards LM3 and LP07 murine cancer cell lines. (C) 2010 Elsevier Masson SAS. All rights reserved.

Luminescence characteristics of YAP:Ce scintillator powders and composites

Cerium doped yttrium aluminate perovskite YAlO(3) (YAP) powders are pursued as interesting alternatives to bulk crystals for application in scintillating devices. The emissions of these materials in the near-UV and visible spectral regions originate from electric dipole transitions between 4f and 5d energy levels of Ce(3+) and largely depend on the environment occupied by the ion. In search for improved synthesis conditions that can lead to phase pure powders with optimized structural and spectroscopic characteristics, in this work we have employed the polymeric precursor (Pechini) method to prepare crystalline and amorphous YAP:Ce powders doped with 1-10 mol% Ce(3+). Interesting composite materials were also obtained by dispersing some of the YAP:Ce powders in silica xerogels. A comparative structural and spectroscopic study of all the samples was done by XRD, FT-IR, emission, excitation and excited state lifetime measurements. In agreement with previous reports, excitation at 296 nm results in intense emission in the range 315-425 nm with an average decay time of 30 ns. (c) 2010 Elsevier B.V. All rights reserved.

Solvothermal Preparation of Drug Crystals: Didanosine

For the first time, crystals of suitable size for X-ray diffractometry structure determination (Dian important anti-HI V drug were prepared under solvothermal conditions. In this study, the crystal structure of didanosine (2`,3`-dideoxyinosine, ddI) in the form of a hydrate was determined using single-crystal X-ray diffractometry. Powder X-ray diffraction analysis revealed that the solid-state phase of the drug incorporated into pharmaceutical solid dosage forms is isostructural to the solvothermally prepared ddI material, even though they do not exhibit an identical chemical composition due to different water fractions occupying hydrophobic channels formed within the crystal lattice. Two ddI conformers are present in the structure, in agreement with a previous structure elucidation attempt. Concerning the keto enol equilibrium of ddI, our crystal data and vibrational characterizations by Fourier transform infrared (FTIR) and FT-Raman spectroscopy techniques were conclusive to state that both conformers exist in the keto form, contrary to solid-state NMR spectroscopic assignments that suggested ddI molecules occur as enol tautomers. In addition, characterizations by thermal (differential scanning calorimetry) and spectroscopic techniques allowed us to understand the structural similarities and the differences related to the hydration pattern of the nonstoichiometric hydrates.

Thermal analysis of prednicarbate and characterization of thermal decomposition product

In the present work, the thermal behavior of prednicarbate was studied using DSC and TG/DTG. The solid product remaining at the first decomposition step of the drug was isolated by TG, in air and N(2) atmospheres and was characterized using LC-MS/MS, NMR, and IR spectroscopy. It was found that the product at the first thermal decomposition step of prednicarbate corresponds to the elimination of the carbonate group bonding to C(17), and a consequent formation of double bond between C(17) and C(16). Structure elucidation of this degradation product by spectral data has been discussed in detail.

V(2)O(5) nanoparticles obtained from a synthetic bariandite-like vanadium oxide: Synthesis, characterization and electrochemical behavior in an ionic liquid

Highly stable and crystalline V(2)O(5) nanoparticles with an average diameter of 15 nm have been easily prepared by thermal treatment of a bariandite-like vanadium oxide, V(10)O(24)center dot 9H(2)O. Their characterization was carried out by powder X-ray diffractometry (XRD). Fourier transform infrared (FT-IR) and Raman spectroscopies, and transmission electron microscopy (TEM). The fibrous and nanostructured film obtained by electrophoretic deposition of the V(2)O(5) nanoparticles showed good electroactivity when submitted to cyclic voltammetry in an ionic liquid-based electrolyte. The use of this film for the preparation of a nanostructured electrode led to an improvement of about 50% in discharge capacity values when compared with similar electrodes obtained by casting of a V(2)O(5) xerogel. (C) 2009 Elsevier Inc. All rights reserved.

Thermal analysis and compatibility studies of prednicarbate with excipients used in semi solid pharmaceutical form

Differential Scanning Calorimetry (DSC), thermogravimetry/derivative thermogravimetry (TG/DTG) and infrared spectroscopy (IR) techniques were used to investigate the compatibility between prednicarbate and several excipients commonly used in semi solid pharmaceutical form. The thermoanalytical studies of 1:1 (m/m) drug/excipient physical mixtures showed that the beginning of the first thermal decomposition stage of the prednicarbate (T (onset) value) was decreased in the presence of stearyl alcohol and glyceryl stearate compared to the drug alone. For the binary mixture of drug/sodium pirrolidone carboxilate the first thermal decomposition stage was not changed, however the DTG peak temperature (T (peak DTG)) decreased. The comparison of the IR spectra of the drug, the physical mixtures and of the thermally treated samples confirmed the thermal decomposition of prednicarbate. By the comparison of the thermal profiles of 1:1 prednicarbate:excipients mixtures (methylparaben, propylparaben, carbomer 940, acrylate crosspolymer, lactic acid, light liquid paraffin, isopropyl palmitate, myristyl lactate and cetyl alcohol) no interaction was observed.

The influence of acetic acid on the ethanol electrooxidation on a platinum electrode

In the presented work, the evaluation of the influence of acetic acid in the electrochemical environment on the ethanol electro-oxidation reaction on a polycrystalline platinum electrode is presented for the first time. Using cyclic voltammetry. chronoamperometry and in situ Fourier Transformed IR spectroscopy (FTIR) it was demonstrated that an inhibition of the ethanol oxidation reaction occurs for bulk acetic acid concentrations of the order 0.1 mu mol L(-1) -5 mmol L(-1). This inhibition effect is related to the decrease of CO(2) and acetaldehyde production as confirmed by spectroscopic results. (C) 2011 Elsevier B.V. All rights reserved.

A surface-enhanced infrared absorption spectroscopic (SEIRAS) study of the oscillatory electro-oxidation of methanol on platinum

The oscillatory electro-oxidation of methanol was studied by means of in situ infrared (IR) spectroscopy in the attenuated total reflection (ATR) configuration using a platinum film on a Si prism as working electrode. The surface-enhanced infrared absorption (SEIRA) effect considerably improves the spectroscopic resolution, allowing at following the coverage of some adsorbing species during the galvanostatic oscillations. Carbon monoxide was the main adsorbed specie observed in the induction period and within the oscillatory regime. The system was investigated at two distinct time-scales and its dynamics characterized accordingly. During the induction period the main transformation observed as the system move through the phase space towards the oscillatory region was the decrease of the coverage of adsorbed carbon, coupled to the increase of the electrode potential. Similar transition characterizes the evolution within the oscillatory region, but at a considerably slower rate. Experiments with higher time resolution revealed that the electrode potential oscillates in-phase with the frequency of the linearly adsorbed CO vibration and that the amount of adsorbed CO oscillates with small amplitude. Adsorbed formate was found to play, if any, a very small role. Results are discussed and compared with other systems. (C) 2010 Elsevier B.V. All rights reserved.

Híbridos à base de anilina/sílica obtidos através do processo sol-gel: síntese, caracterização e propriedades

Neste trabalho inicialmente foi sintetizado o precursor organoalcoxisilano 3- anilinapropiltrimetoxisilano, APTMS, a partir da reação entre a anilina e o 3- cloropropiltrimetoxisilano, CPTMS, usando hidreto de sódio, NaH, como ativador de base. O precursor inorgânico tetraetilortosilicato, TEOS, foi polimerizado na presença do precursor orgânico, e catalisador. Durante a etapa de polimerização dos precursores alcóxidos, foram investigadas as influências da temperatura, do tipo e concentração do catalisador e da concentração de precursor orgânico adicionado nas propriedades finais dos híbridos anilinapropilsilica resultantes. Os materiais híbridos foram caracterizados através das técnicas: espectroscopia no infravermelho (FT-IR), técnica de espalhamento de Raios-x a baixos ângulos (SAXS), microscopia eletrônica de varredura (SEM), isotermas de adsorção e dessorção de nitrogênio, análise elementar, espectroscopia de aniquilação de pósitrons (PALS), análise termogravimétrica (TGA), espectroscopia de elétrons dispersos (EDS). A potencialidade de aplicação dos híbridos obtidos como materiais adsorventes na extração dos cátions Cu(II), Zn(II), Cd(II) e Co(II), em solução, foi investigada usando-se isotermas de adsorção pelo método batelada. Através das técnicas de caracterização foi possível observar que as propriedades morfológicas dos materiais como área superficial, distribuição do tamanho de poros, forma e tamanho das partículas, além da estabilidade e grau de incorporação orgânica podem ser controladas em maior ou menor grau, dependendo da variável usada durante a polimerização dos precursores alcóxidos. O material apresentou propriedades promissoras como adsorvente seletivo para o cobre.

Evaluation of the zinox and zeolite materials as adsorbents to remove H2S from natural gas

MELO, Dulce Maria de Araújo et al. Evaluation of the Zinox and Zeolite materials as adsorbents to remove H2S from natural gas. Colloids and Surfaces. A, Physicochemical and Engineering Aspects, Estados Unidos, v. 272, p. 32-36, 2006.

Efeito de glucanas do fungo Caripia montagnei em modelo de inflamação intestinal induzida por tnbs em ratos Wistar e em células de carcinoma de cólon humano HT-29

Compounds derived from fungi has been the subject of many studies in order to broaden the knowledge of their bioactive potential. Polysaccharides from Caripia montagnei have been described to possess anti-inflammatory and antioxidant properties. In this study, glucans extracted from Caripia montagnei mushroom were chemically characterized and their effects evaluated at different doses and intervals of treatment. It was also described their action on colonic injury in the model of colitis induced by 2,4,6-trinitrobenzene sulfonic acid (TNBS), and its action on cells of the human colon carcinoma (HT-29). Compounds extracted of C. montagnei contain high level of carbohydrates (96%), low content of phenolic compounds (1.5%) and low contamination with proteins (2.5%). The (FT-IR) and (NMR) analysis showed that polysaccharides from this species of mushroom are composed of α- and β-glucans. The colonic damage was evaluated by macroscopic, histological, biochemical and immunologic analyses. The results showed a reduction of colonic lesions in all groups treated with the glucans of Caripia montagnei (GCM). GCM significantly reduced the levels of IL-6 (50 and 75 mg/kg, p < 0.05), a major inflammatory cytokine. Biochemical analyses showed that such glucans acted on reducing levels of alkaline phosphatase (75 mg/kg, p < 0.01), nitric oxide (p < 0.001), and myeloperoxidase (p < 0.001). These results were confirmed microscopically by the reduction of cellular infiltration. The increase of catalase activity suggest a protective effect of GCM on colonic tissue, confirming their anti-inflammatory potential. GCM displayed cytostatic activity against HT-29 cells, causing accumulation of cells in G1 phase, blocking the cycle cell progression. Those glucans also showed ability to modulate the adhesion of HT-29 cells to Matrigel® and reduced the oxidative stress. The antiproliferative activity against HT-29 cells displayed by GCM (p <0.001) can be attributed to its cytostatic activity and induction of apoptosis by GCM

Polissacarídeos sulfatados da Alga Marrom Dictyopteris justii como agentes antioxidantes e inibidores da formação de cristais de oxalato de cálcio

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Adsorção de Pb(II) utilizando adsorvente composto por montmorilonita e dolomita

The destructive impact of improper disposal of heavy metals in the environment increases as a direct result of population explosion, urbanization and industrial expansion and technological developments. Argil are potential materials for adsorption of inorganic and the pelletization of it is required for use in adsorptive columns of fixed bed. The low cost and the possibility of regeneration makes these materials attractive for use in the purification process, capable of removing inorganic compounds in contaminated aquatic environments. In this work was made pellets of a mixture of dolomite and montmorillonite by wet agglomeration, in different percentages. The removal of Pb (II) was investigated through experimental studies, and was modeled by kinetic models and isotherms of adsorption. The materials were characterized using the techniques of XRD, TG / DTA, FT-IR, and surface area by BET method. The results showed the adsorption efficiency of the contaminant by the composite material studied in synthetic solution. The study found that the adsorption follows the Langmuir model, and the kinetics of adsorption follows the model of pseudosecond order

Síntese de zeólita A a partir de diatomita como fonte de aluminossilicato

The synthesis of zeolites from natural sources of silicon and aluminum are promising alternative routes to obtain porous or zeolite MCM family. Such materials are typically used in catalytic processes and / or adsorption is to obtain new products or for separation and purification processes thereof. Environmental legislation is becoming stricter and requires the use of materials more efficient, aiming to achieve pollution prevention, by gas or liquid contaminants in the environment. In order to obtain a material with environmentally friendly features, this study aimed at the synthesis of zeolite A, from an amorphous sediment, diatomite, which is found in abundance in the northeast region of Brazil, may be substituted for conventional products the production of zeolite, involving higher costs. The methodology for obtaining the "Zeolite A" using as a source of silica and alumina diatomite is simple, since this is a source of silicon, not requiring therefore a structural driver, but also by heat treatment, only drying conventional to remove water. The "zeolite A" was obtained from diatomite, but as an intermediate step we obtained the sodalite. The characterization was made by the following techniques: EDX, XRD, FT-IR, SEM and determining a specific area by the BET method and the BJH method for checking the diameter of pores. By characterization of the obtained material was first demonstrated the achievement of sodalite and after modification of the same, there was obtained zeolite A

Adição de resíduo cerâmico em pastas geopoliméricas para cimentação de poços de petróleo

The development of activities the of oil and gas sector have promoted the search for suitable materials for cementing oil wells. In the state of the Rio Grande do Norte, the integrity of the cement sheath tends to be impaired during steam injection, a procedure necessary to increase oil recovery in reservoirs with low-viscosity oil. The geopolymer is a material that can be used as alternative cement, since it has been used in the production of fire-resistant components, building structures, and for the control of toxic or radioactive residues. Geopolymers result from condensation polymer alkali aluminosilicates and silicates resulting three-dimensional polymeric structures. They are produced in a manner different from that of Portland cement, which is made an activating solution that is mixed with geopolymer precursor. Among the few works studied allowed us to conclude that the pastes prepared with metakaolin as precursor showed better performance of its properties. Several studies show the addition of waste clay as a means of reducing cost and improving end of the folder properties. On this basis, the goal is to study the influence of the addition of ceramic waste in geopolymer paste. To develop the study of rheology tests were carried out, filtered, thickening time, compressive strength, free water, specific gravity and permeability, according to the American Pretoleum Institute (API). The results for all formulations studied show that the folders have high mechanical strength to a light paste; low filtrate volume, absence of free water, very low permeability, slurry, consistent with a light paste, and thickening time low that can be corrected with the use of a retardant handle. For morphological characterization, microstructural, physical, chemical and thermal tests were carried out by XRD, MEV, DTA, TG, FTIR. In the trial of XRD, it was found that geopolymer is an amorphous material, with a peak of crystalline kaolinite. In tests of TG / DTA, revealed the presence of a significant event, which represents the mass loss related to water, and also observed the reduction of weight loss by increasing the concentration of ceramic waste. In the trial of MEV, we found a uniform matrix without the presence of other phases. In the trial of FT-IR, we observed the presence of the band related to water. From all results it was determined that the optimum concentration range of use is between 2.5 and 5% of waste ceramic