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91.
Lefebvre BG Liu W Peterson RW Valentine KG Wand AJ 《Journal of magnetic resonance (San Diego, Calif. : 1997)》2005,175(1):158-162
Traditionally, large proteins, aggregation-prone proteins, and membrane proteins have been difficult to examine by modern multinuclear and multidimensional solution NMR spectroscopy. A major limitation presented by these protein systems is that their slow molecular reorientation compromises many aspects of the more powerful solution NMR methods. Several approaches have emerged to deal with the various spectroscopic difficulties arising from slow molecular reorientation. One of these takes the approach of actively seeking to increase the effective rate of molecular reorientation by encapsulating the protein of interest within the protective shell of a reverse micelle and dissolving the resulting particle in a low viscosity fluid. Since the encapsulation is largely driven by electrostatic interactions, the preparation of samples of acidic proteins suitable for NMR spectroscopy has been problematic owing to the paucity of suitable cationic surfactants. Here, it is shown that the cationic surfactant CTAB may be used to prepare samples of encapsulated anionic proteins dissolved in low viscosity solvents. In a more subtle application, it is further shown that this surfactant can be employed to encapsulate a highly basic protein, which is completely denatured upon encapsulation using an anionic surfactant. 相似文献
92.
James F. Sanders John D. Ferry Robert H. Valentine 《Journal of Polymer Science.Polymer Physics》1968,6(5):967-980
Viscoelastic properties of uncrosslinked 1,2-polybutadiene (91.5% vinyl, 7.0% cis, 1.5% trans, number-average molecular weight 99,000) were studied by dynamic shear measurements between 0.15 and 600 cps (torsion pendulum and Fitzgerald transducer) and shear creep measurements over time periods up to 3.7 × 104 sec., in the temperature rang from 5 to 50°C. More limited dynamic measurements were made on a sample of unvulcanized natural rubber with number-average molecular weight 350,000 at frequencies from 0.4 to 400 cps and temperatures from 13 to 48°C. All data were reduced to 25°C. by shift factors calculated from equations of the WLF form with the following coefficients: 1,2-polybutadiene, c1 = 6.23, c2 = 72.5; natural rubber, c1 = 5.94, c2 = 151.6. In the transition zone, the relative positions of the loss tangent curves on the logarithmic frequency scale for these and other rubbers (1,4-polybutadiene with 50% trans configuration; styrene–butadiene rubber with 23.5% styrene content; and polyisobutylene) provided relative measures of local segment mobility. At 25°C., these ranged over a factor of 3700 with 1,2-polybutadiene and polyisobutylene the lowest and 1,4-polybutadiene the highest. When the frequency scale of each rubber was reduced to a temperature 100°C. above its glass transition temperature, however, the loss tangent curves for all except polyisobutylene were nearly coincident; the latter still showed a lower mobility by a factor of about 1/800. The terminal relaxation time and steady-state compliance for the 1,2-polybutadiene calculated from the Rouse theory were larger than those observed experimentally. The level of compliance corresponding to the entanglement network of 1,2-polybutadiene, JeN, was calculated by integration over the loss compliance, J″, to be 1.62 × 10?7 cm.2/dyne; integration over G″ to obtain the corresponding modulus gave reasonable agreement. From such JeN, values, the average number of chain atoms between entanglement points, jZe, was estimated as follows: 1,2-polybutadiene, 132; natural rubber, 360; 1,4-polybutadiene, 110; styrene–butadiene rubber, 186; polyisobutylene, 320. Values of jZe were also estimated from the minimum in the loss tangent and compared with those reported from the molecular weight dependence of viscosity. The three sources were in generally good agreement. 相似文献
93.
94.
Prof. Dr. Valentine G. Nenajdenko Dr. Aleksey A. Goldberg Dr. Vasily M. Muzalevskiy Prof. Dr. Elizabeth S. Balenkova Dr. Aleksey V. Shastin 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(7):2370-2383
A convenient and simple three‐step pathway to the new family of CF2CF2S‐bridged alkanes and CF2S‐, CF2O‐bridged alkenes and alkynes was elaborated by using catalytic olefination reaction as a key step of the synthetic sequence. The obtained compounds revealed attractive liquid crystalline characteristics. 相似文献
95.
Yury Yu. Rusakov Leonid B. Krivdin Nikolay V. Orlov Valentine P. Ananikov 《Magnetic resonance in chemistry : MRC》2011,49(9):570-574
Stereochemical study of five sterically crowded phenylselanylalkenes obtained via the hydroselenation of either terminal or internal alkynes with benzeneselenol catalyzed by the nanosized Ni complexes has been carried out based on the experimental HMBC measurements and theoretical second order palarization propagator approach (SOPPA) calculations of their 77Se? 1H spin–spin coupling constants across double bond in combination with the energy‐based theoretical conformational analysis performed at the MP2/6‐311G** level. It has been found that studied phenylselanylalkenes adopt mainly skewed s‐cis conformation with the noticeable out‐of‐plane deviations of the phenylselanyl and phenyl groups. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
96.
Vassiliki Theodorou Marina GogouMaria Philippidou Valentine RagoussisGeorgios Paraskevopoulos Konstantinos Skobridis 《Tetrahedron》2011,67(31):5630-5634
α,β-Unsaturated acids, through their acid chlorides, react with tritylamine in the presence of triethylamine under mild conditions, to afford in high yield and high regioselectivity the corresponding β,γ-unsaturated tritylamides. Detritylation with TFA generates quantitatively β,γ-unsaturated primary amides. An investigation of this deconjugative isomerization was performed. 相似文献
97.
Comte Fabienne Genon-Catalot Valentine 《Statistical Inference for Stochastic Processes》2021,24(1):149-177
Statistical Inference for Stochastic Processes - We consider a Gaussian continuous time moving average model $$X(t)=\int _0^t a(t-s)dW(s)$$ where W is a standard Brownian motion and a(.) a... 相似文献
98.
Li Y Chooi YH Sheng Y Valentine JS Tang Y 《Journal of the American Chemical Society》2011,133(39):15773-15785
99.
Ahmad Kiani Karanji Maryssa Beasley Daud Sharif Ali Ranjbaran Justin Legleiter Stephen J. Valentine 《Journal of mass spectrometry : JMS》2020,55(1)
The first 17 amino acid residues of Huntingtin protein (Nt17 of htt) are thought to play an important role in the protein's function; Nt17 is one of two membrane binding domains in htt. In this study the binding ability of Nt17 peptide with vesicles comprised of two subclasses of phospholipids is studied using electrospray ionization ‐ mass spectrometry (ESI‐MS) and molecular dynamics (MD) simulations. Overall, the peptide is shown to have a greater propensity to interact with vesicles of phosphatidylcholine (PC) rather than phosphatidylethanolamine (PE) lipids. Mass spectra show an increase in lipid‐bound peptide adducts where the ordering of the number of such specie is 1,2‐dioleoyl‐sn‐glycero‐3‐phosphocholine (DOPC) > 1‐palmitoyl‐2‐oleoyl‐glycero‐3‐phosphocholine (POPC) > 1‐palmitoyl‐2‐oleoyl‐sn‐glycero‐3 phosphoethanolamine (POPE). MD simulations suggest that the compactness of the bilayer plays a role in governing peptide interactions. The peptide shows greater disruption of the DOPC bilayer order at the surface and interacts with the hydrophobic tails of lipid molecules via hydrophobic residues. Conversely, the POPE vesicle remains ordered and lipids display transient interactions with the peptide through the formation of hydrogen bonds with hydrophilic residues. The POPC system displays intermediate behavior with regard to the degree of peptide‐membrane interaction. Finally, the simulations suggest a helix stabilizing effect resulting from the interactions between hydrophobic residues and the lipid tails of the DOPC bilayer. 相似文献
100.
Mahdiar Khakinejad Samaneh Ghassabi Kondalaji Hossein Maleki James R. Arndt Gregory C. Donohoe Stephen J. Valentine 《Journal of the American Society for Mass Spectrometry》2014,25(12):2103-2115
The gas-phase conformations of electrosprayed ions of the model peptide KKDDDDIIKIIK have been examined by ion mobility spectrometry (IMS) and hydrogen deuterium exchange (HDX)-tandem mass spectrometry (MS/MS) techniques. [M+4H]4+ ions exhibit two conformers with collision cross sections of 418 Å2 and 471 Å2. [M+3H]3+ ions exhibit a predominant conformer with a collision cross section of 340 Å2 as well as an unresolved conformer (shoulder) with a collision cross section of ~367 Å2. Maximum HDX levels for the more compact [M+4H]4+ ions and the compact and partially-folded [M+3H]3+ ions are ~12.9, ~15.5, and ~14.9, respectively. Ion structures obtained from molecular dynamics simulations (MDS) suggest that this ordering of HDX level results from increased charge-site/exchange-site density for the more compact ions of lower charge. Additionally, a new model that includes two distance calculations (charge site to carbonyl group and carbonyl group to exchange site) for the computer-generated structures is shown to better correlate to the experimentally determined per-residue deuterium uptake. Future comparisons of IMS-HDX-MS data with structures obtained from MDS are discussed with respect to novel experiments that will reveal the HDX rates of individual residues. Graphical Abstract
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