975 resultados para C-13 and 2D NMR


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Octakis(cyanopropyldimethylsiloxy)octasilsesquioxane was prepared and characterized by C-13, Si-29 NMR (MAS), SEM, FF-IR, XRD and thermogravimetric techniques. The four groups alpha, beta, gamma, kappa (to the terminal silicon atom), associated with an acrylonitrile, were clearly seen in the C-13 NMR (alpha-CH2 at 17.9; P-CH2 at 31.3; gamma-CH, at 50.4; K-C N at 59.0 ppm). The Si-29 NMR spectrum of the final product, exhibits only Q type silicon signal, ascribed to Q(4) (-118.0 ppm). The presence of acrylonittile substituted for octameric cube confers a relative change phase and thermal stability to the material. With regard to the applications for this new material, it was intended, in this case, to react with Na-2[Fe(CN)(5)NH3] by chemical substitution. This composite was incorporated into a carbon paste electrode and the electrochemical studies were performed by cyclic voltammetry. The cyclic voltammogram of the modified graphite paste electrode, showed one redox couples with formal potential (E-1/2(ox)) = 0.24 V versus SCE. (c) 2006 Elsevier B.V. All rights reserved.

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In this work we report on new optically pumped THz laser lines from deuterated formic acid (DCOOD). An isotopic (CO2)-C-13 laser was used for the first time as a pump source for this molecule, and a Fabry-Perot cavity was used as a THz laser resonator. Optoacoustic absorption spectra were used as a guide to search for new THz laser lines. We could observe six new laser lines in the range from 303.8 mu m (0.987 THz) to 725.1 mu m (0.413 THz). The lines were characterized according to wavelength, relative polarization, relative intensity, and optimum working pressure. The transferred lamb-dip technique was used to measure the frequency absorption transition for both of these laser lines. Furthermore, we also present a catalogue of all THz laser lines generated from DCOOD.

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The effects of grain-based diets from C3 or C4-cycle plants on muscle delta C-13 change process in Nile tilapia (Oreochromis niloticus) fingerlings were investigated. Two groups of sex reversal males Nile tilapia fingerlings were fed with isoproteic (32.0% DP) and isocaloric (3200 kcal DE/kg) diets, differing from each other by their delta C-13. Muscle samples were collected and the carbon isotopic composition was measured. For C4 diet, the formula for the muscle delta C-13 change related to the intake time of a new diet was delta C-13=- 14.88 - 9.2 1 e(-0.0209t) and the half-life (T) of the muscle carbon was 33.2 days. For C3 diet, the formula was delta C-13 = - 25.43 + 8.59e(-0.0533), with T = 13 days. The C3 diet was considered more appropriate based on its palatability and consequent larger food intake than the C4 diet, resulting in an increased muscle delta C-13 change rate. However, for future studies, would be necessary to mix both the C3 and C4 feedstuffs to formulate diets nutritionally appropriated, with contrasting stable isotopes signatures. Tissue delta C-13 change rate is therefore indicated as a promising tool to better understand the biotic and abiotic factors that influence nutrients utilization from the diet and animal growth. (c) 2006 Elsevier B.V. All rights reserved.

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A myeloperoxidase inhibitory kaempferol derivative, namely pterogynoside (1), was isolated from fruits of Pterogyne nitens, along with six known flavonols, kaempferol, afzelin, kaempferitrin, quercetin, isoquercetrin and rutin. The structures of all compounds were elucidated primarily from 1D and 2D NMR spectroscopic analyses, as well as by high resolution mass spectrometry. All flavonols were screened to identify secondary metabolites as potential myeloperoxidase (MPO) inhibitors, and at concentrations of 0.50-50 nM, quercetin (5), isoquercitrin (6) and rutin (7) exhibited strong inhibitory effects with IC(50) values of 1.22 +/- 0.01, 3.75 +/- 0.02 and 3.60 +/- 0.02, respectively. The MPO activity detected for the new derivative 1 was markedly decreased (IC(50) 10.3 +/- 0.03) when compared with known flavonols 5-7, and interestingly increased when tested against ABTS scavenging activity. (C) 2008 Published by Elsevier Ltd.

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8-Carboxymethyl-1,6-dihydroxy-3,5-dimethoxyxanthone 8-carboxymethyl-1,5,6-trihydroxy-3-methoxyxanthone and 8-carboxy-methyl-1,3,5,6-tetrahydroxyxanthone were isolated from the capitula of Leiothrix curvifolia and Leiothrix flavescens and characterized by spectroscopic methods, mainly 1D and 2D NMR experiments, as well as by electrospray mass spectrometry. Eight known flavonoids were also isolated and they were identified by 1D and 2D NMR experiments and comparison with literature data. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

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Aqueous infusions of Brazilian Maytenus leaves are used as beverages, foodstuffs, and phytomedicines. Previously, we isolated two new flavonoid tetrasaccharides from the infusion of Maytenus aquifolium leaves that showed antiulcer activity. In this investigation a new flavonoid tetrasaccharide, kaempferol-3-O-alpha -L-rhamnopyranosyl (1-6)-O-[alpha -L-arabinopyranosyl (1 -->3)-O-alpha -L-rhamnopyranosyl (1-2)]-O-beta -D-galactopyranoside (3), was isolated, together with kaempferol tri- and disaccharides and quercetin trisaccharides from the aqueous infusion of Maytenus ilicifolia leaves. All structures were elucidated by ES-MS and NMR spectroscopic methods. The quantitative analysis of the flavonoid glycosides from Maytenus ilicifolia and M. aquifolium has been performed by HPLC.

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The effects of 200 mM copper ions on the synthesis of membrane and periplasmic proteins were investigated in iron-grown cells of Acidithiobacillus ferrooxidans (At. ferrooxidans). Total membrane protein profiles of cells grown in the absence of copper ions (unadapted cells) and in the presence of copper ions (copper-adapted cells) were compared by two-dimensional polyacrylamide gel electrophoresis (2D-PAGE). Crude preparations of outer membrane and periplasmic proteins were analyzed by SDS-PAGE. The synthesis of proteins was diminished or increased in the presence of copper ions. Low molecular weight proteins (< 14 kDa) were significantly repressed by copper. These proteins are probably acidic proteins located in the outer membrane. An over-expression of a periplasmic protein of about 17 kDa was detected in the copper-adapted cells and was assumed to be rusticyanin, a 16.5-kDa periplasmic copper protein present in At. ferrooxidans cells and involved in the electron-transport chain of the iron oxidation pathway. To our knowledge, this is the first report of a possible involvement of the rusticyanin and outer membrane proteins in the mechanism of copper resistance in At. ferrooxidans. (C) 2003 Elsevier B.V. All rights reserved.

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We report the synthesis and characterization of organic-inorganic hybrid materials: Zn-2-Al-LDHs (layered double hydroxides) containing 3-(1H-pyrrol-1-yl)-propanoate and 7-(1H-pyrrol-l-yl)-heptanoate as the interlayer anions. The LDHs were synthesized by the co-precipitation method at constant pH followed by hydrothermal treatment for 72 h. The materials were characterized by PXRD, C-13 CP-MAS NMR, TGA, and ESR. The basal spacing found by PXRD technique is coincident with the formation of bilayers of the intercalated anions. The solid state C-13 NMR showed that the interlayered anions remain identical after intercalation. ESR data suggest that the monomers connect each other in a limited number of guests when a thermal treatment is applied. The inorganic LDH sheets delay the temperature of degradation of the monomers. (c) 2006 Elsevier Ltd. All rights reserved.

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Droplet countercurrent chromatography and high-performance liquid chromatography fractionation of the aqueous infusion from Maytenus aquifolium Martius leaves afforded two flavonoid tetrasaccharides: quercetin 3-O-alpha-L-rhamnopyranosyl(1-->6)-O-[beta-D-glucopyranosyl(1-->3)-O-alpha-L-rhamnopranosyl( 1-->2)-O-beta-D-galactopyranoside and kaempferol 3-O-alpha-L-rhamnopyranosyl(1-->6)-O-[beta-D-glucopyranosyl( 1-->3)-O-alpha-L-rhamnopyranosy(1-->2-2)-O-beta-D-galactopyranoside. All structures were elucidated by spectroscopic methods. Pharmacological essays of the infusion showed antiulcer activity in rats.