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[reaction: see text] The syntheses of 4,4a-didehydrohimbacine and 4,4a-didehydrohimandravine are presented. Key steps include an intramolecular Diels-Alder reaction of a bromopentadienyl acrylate and Suzuki-Miyaura and Stille coupling reactions. 相似文献
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Natacha Lourette Heather Smallwood Si Wu Errol W. Robinson Thomas C. Squier Richard D. Smith Ljiljana Paša-Tolić 《Journal of the American Society for Mass Spectrometry》2010,21(6):930-939
A liquid chromatography-mass spectrometry (LC-MS)-based approach for characterizing the degree of nitration and oxidation of intact calmodulin (CaM) has been used to resolve ~250 CaM oxiforms using only 500 ng of protein. The analysis was based on high-resolution data of the intact CaM isoforms obtained by Fourier-transform ion cyclotron resonance mass spectrometry (FTICR MS) coupled with an on-line reversed-phase LC separation. Tentative identifications of post-translational modifications (PTMs), such as oxidation or nitration, have been assigned by matching observed protein mass to a database containing all theoretically predicted oxidation products of CaM and verified through a combination of tryptic peptide information (generated from bottom-up analyses) and on-line collisionally induced dissociation (CID) tandem mass spectrometry (MS/MS) at the intact protein level. The reduction in abundance and diversity of oxidatively modified CaM (i.e., nitrated tyrosines and oxidized methionines) induced by macrophage activation has been explored and semiquantified for different oxidation degrees (i.e., no oxidation, moderate, and high oxidation). This work demonstrates the power of the top-down approach to identify and quantify hundreds of combinations of PTMs for single protein target such as CaM and implicate competing repair and peptidase activities to modulate cellular metabolism in response to oxidative stress. 相似文献
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Five butane-2,3-diacetals obtained from the reaction of 1,2-diols and methanol with biacetyl have been treated with allylsilane in the presence of titanium tetrachloride to afford bis-allyldioxanes as single diastereoisomers. 相似文献
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This work focuses on interstitial solid solutions of hydrogen in the face-centred cubic (fcc) host lattice of palladium and nickel, using a first-principles based approach. Cluster Variation Method (CVM) and Monte Carlo simulation algorithms were especially designed, allowing a coupled use of both techniques, to study hydrogen–vacancy interactions inside an fcc metallic host lattice. First-principles calculations provided the H–Vac interaction energies by structure inversion method. The phase diagrams and thermodynamic properties were computed using only theoretical inputs. The mechanisms leading to the formation of the miscibility gaps observed for both Pd–H and Ni–H systems and the hydrogen ordering on palladium interstitial lattice were reproduced without any empirical term. 相似文献
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Pedro Rocha ngela Vilas‐Boas Natacha Fontes Dulce Geraldo Ftima Bento 《Electroanalysis》2020,32(1):159-165
The electrochemical oxidation processes that occur during a voltammetric assay in wine samples lead to the formation of species that obstructs the surface and reduce their active area. This effect is critical for screen printed carbon electrodes (SPCE) and leads to abnormal low values of the total polyphenols content of wines, ca. 72 % lower than those obtained with glassy carbon electrodes. This effect was examined using 10 red and Port wine samples. Mechanical polishing and electrochemical‐based treatments for the removal of this fouling layer were tested. The best results were obtained by electrochemical activation in at a constant potential of 1.2 V during 100 s Na2CO3 saturated solution, and by polishing. The success of some of these treatments brings an added value to SPCE, as it opens the possibility of their reuse in the wine analysis. This outcome is particularly relevant for quality control where a huge number of analysis is performed and the reduction of cost may dictates the choice of the analytical method. 相似文献
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We report how the control of a single parameter, the co-surfactant, determines the phase transitions of oil-in-water swollen liquid crystals (SLCs) prepared with cetyltrimethylammonium bromide (CTAB), from cubic to hexagonal, lamellar, and finally sponge-like structures. SLCs are complex mixtures (surfactant + co-surfactant + water + salt + oil) usually prepared to form hexagonal mesophases, with cell parameters tunable between 3 and 30 nm. These hexagonal mesophases were successfully used as nanoreactors to prepare a broad range of nanostructured materials. Because the potential of these mesophases as adaptive nanoreactors has not been extended to other liquid crystal geometries than the hexagonal, we studied in a first step the structure evolution of SLCs made with CTAB, cyclohexane, pentanol-1, water and different stabilising salts. We used small-angle X-ray scattering (SAXS), polarised light microscopy and Freeze-Fracture TEM to provide a partial phase diagram and list the different mesophases obtained as a function of composition. We report that the adjustment of a single parameter, the co-surfactant (pentanol-1), determines the phase transition between cubic, hexagonal, lamellar, and sponge-like structures, all other parameters such as the nature and concentration of salt, or amount of oil being constant. 相似文献