71 resultados para bidimensional NMR

em Repositório Institucional UNESP - Universidade Estadual Paulista "Julio de Mesquita Filho"


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O fracionamento cromatográfico do extrato etanólico das folhas de Nectandra grandiflora resultou no isolamento de dois flavonóides glicosilados que apresentaram atividade antioxidante inibindo a oxidação do beta -caroteno em CCDC. As substâncias isoladas tiveram suas estruturas elucidadas através de técnicas espectrométricas de RMN uni- e bidimensional e foram identificadas como 3-O-beta -ramnosy kaempferol and 3-O-beta -ramnosylquercetina.

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Ceftazidime shows two main polarographic reduction peaks at pH 4.0, that at -0.45 V owing to reduction of the C=N bond in the methylethoxyimino group and that at -1.00 V owing to the reductive elimination of pyridine: the first peak is particularly suitable for the determination of ceftazidime. Ceftazidime can also be determined indirectly using the tensammetric peak at -0.60 V (in Britton-Robinson buffer pH 9.5) of pyridine liberated on hydrolysis. Ceftazidime can be determined in urine using the direct method only after Cls solid phase extraction, but it can be determined directly in the urine by hydrolysing it and using the pyridine peak. (C) 1997 Elsevier B.V. B.V.

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Remazol brilliant orange 3R shows only a voltammetric peak for the reduction of the azo group. No peak was observed for the reduction of the sulfatoethylsulfone or vinylsulfone reactive groups. The reduction of a pre-protonated ate group involving a two-electron process, gives a hydrate derivative in acidic solution. In alkaline solution the reduction process occurs at more negative potential with the formation of an unstable hydrate compound which decomposes via HN-NH bond cleavage and loss of a sulfate group. Optimum conditions are given for the cathodic stripping voltammetric determination of dir: dye in aqueous solution. The optimum accumulation potential and time were 0 V and up to 60 s, respectively. Linear calibration graphs were obtained from 30 to 300 ng ml(-1) in pH 4 and 6.2 to 62 ng ml(-1) in pH 10. The limit of determination obtained was 1.5 ng ml(-1) (pH 10). The coefficient of variation was 2.6% (n = 7) at 62 ng ml(-1) of the reactive dye. (C) 1999 Elsevier B.V. B.V. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Pós-graduação em Biofísica Molecular - IBILCE

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We have examined the effect of the uncharged species of lidocaine (LDC) and etidocaine (EDC) on the acyl chain moiety of egg phosphatidylcholine liposomes. Changes in membrane organization caused by both anesthetics were detected through the use of EPR spin labels (5, 7 and 12 doxyl stearic acid methyl ester) or fluorescence probes (4, 6, 10, 16 pyrene-fatty acids). The disturbance caused by the LA was greater when the probes were inserted in more external positions of the acyl chain and decreased towards the hydrophobic core of the membrane. The results indicate a preferential insertion of LDC at the polar interface of the bilayer and in the first half of the acyl chain, for EDC. Additionally, 2 H NMR spectra of multilamellar liposomes composed by acyl chain-perdeutero DMPC and EPC (1:4 mol%) allowed the determination of the segmental order (S-mol) and dynamics (T-1) of the acyl chain region. In accordance to the fluorescence and EPR results, changes in molecular orientation and dynamics are more prominent if the LA preferential location is more superficial, as for LDC while EDC seems to organize the acyl chain region between carbons 2-8, which is indicative of its positioning. We propose that the preferential location of LDC and EDC inside the bilayers creates a "transient site", which is related to the anesthetic potency since it could modulate the access of these molecules to their binding site(s) in the voltage-gated sodium channel. (C) 2007 Elsevier B.V. All rights reserved.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Quantum mechanics calculations at the ab initio HF/3-21G* level were carried out with Nuclear Magnetic Resonance (NMR) measurements to characterize citric acid and lithium interactions. The results indicate the formation of a tridentate organometallic compound with one lithium and one citric acid molecule and a tridentate and bidentate compound of two lithium atoms and one citric acid molecule. The results are in agreement with the experimental and theoretical data. (C) 1999 Elsevier B.V. B.V. All rights reserved.

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Low molecular weight fractions of polyisoprene extracted from Ficus elastica Herb. ex Hornem. were studied by C-13-NMR. The identification of 2-3 trans terminal units at the end of the polymer chain needed the acquisition of more than 17 000 transients. (C) 2000 Elsevier B.V. Ltd. All rights reserved.

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Electrical conductivity and H-1 Nuclear Magnetic Resonance (NMR) techniques were used to investigate the ion-exchanged layered lead-niobate perovskite HPb2Nb3O10. nH(2)O, over the temperature range 90-350 K. Compounds were synthesized by the sol-gel method and calcinated at 650 degreesC. Analysis of the NMR data gives activation energies for the proton motion in the range 0.14-0.40 eV, which are dependent on the water content. The frequency and temperature dependencies of the proton spin-lattice relaxation times show that the character of the motion of the: water molecules is essentially two-dimensional, reflecting the layered structure of the material. The H-1 line-narrowing transition and the single spin-lattice relaxation rate maximum, observed in the hydrated compounds, are consistent with a Grotthuss-like mechanism for the proton diffusion. (C) 2000 Elsevier B.V. B.V. All rights reserved.

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Elemental composition and spectroscopic properties (FT-IR and CP/MAS C-13-NMR) of sedimentary humic substances (HS) from aquatic subtropical environments (a lake, an estuary and two marine sites) are investigated. Humic acids (HA) are relatively richer in nitrogen and in aliphatic chains than fulvic acids (FA) from the same sediments. Conversely, FA are richer in carboxylic groups and in ring polysaccharides than HA. Nitrogen is mostly present as amide groups and for lake and marine HS the FT-IR peaks around 1640 cm(-1) and 1540 cm(-1) identify polypeptides. Estuarine HS exhibit mixed continental-marine influences, these being highly influenced by site location. Overall, the data suggest that aquatic and mixed HS are more aliphatic than has been proposed in current models and also that amide linkages form an important part of their structural configuration.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)