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101.
Zhengtian T. Gu Stanley J. Opella 《Journal of magnetic resonance (San Diego, Calif. : 1997)》1999,140(2):340
Two-dimensional 1H/13C polarization inversion spin exchange at the magic angle experiments were applied to single crystal samples of amino acids to demonstrate their potential utility on oriented samples of peptides and proteins. High resolution is achieved and structural information obtained on backbone and side chain sites from these spectra. A triple-resonance experiment that correlates the 1H–13Cα dipolar coupling frequency with the chemical shift frequencies of the α-carbon, as well as the directly bonded amide 15N site, is also demonstrated. In this experiment the large 1H–13Cα heteronuclear dipolar interaction provides an independent frequency dimension that significantly improves the resolution among overlapping 13C resonances of oriented polypeptides, while simultaneously providing measurements of the 13Cα chemical shift, 1H–13C dipolar coupling, and 15N chemical shift frequencies and angular restraints for backbone structure determination. 相似文献
102.
Swapna GV Montelione GT 《Journal of magnetic resonance (San Diego, Calif. : 1997)》1999,137(2):437-442
Short transverse relaxation times of Calpha and Cbeta single-quantum coherences reduce the sensitivity of triple-resonance experiments involving transfers of Calpha/Cbeta or Halpha/Hbeta coherences. Multiple-quantum line-narrowing techniques improve the relaxation properties of 13C coherences, thereby increasing the sensitivity of the experiment. In the present work, we describe PFG-CBCA(CO)NH and PFG-HBHA(CO)NH experiments that utilize heteronuclear multiple-quantum coherences in a simultaneous constant-time period to obtain completely decoupled spectra with improved sensitivity. Results indicate that approximately 30% of cross peaks show an average enhancement of approximately 15% in the CBCA(CO)NH experiment. In the related HBHA(CO)NH experiment, approximately 97% of the cross peaks show an average enhancement of approximately 40%. 相似文献
103.
A. Krushelnitsky D. Reichert G. Hempel V. Fedotov H. Schneider L. Yagodina A. Schulga 《Journal of magnetic resonance (San Diego, Calif. : 1997)》1999,138(2):244-255
Superslow backbone dynamics of the protein barstar and the polypeptide polyglycine was studied by means of a solid-state MAS 1D exchange NMR method (time-reverse ODESSA) that can detect reorientation of nuclei carrying anisotropic chemical shift tensors. Experiments were performed on carbonyl 13C in polyglycine (natural abundance) and backbone 15N nuclei in uniformly 15N-enriched barstar within a wide range of temperatures in dry and wet powders for both samples. Two exchange processes were observed in the experiments: molecular reorientation and spin diffusion. Experimental conditions that are necessary to separate these two processes are discussed on a quantitative level. It was revealed that the wet protein undergoes molecular motion in the millisecond range of correlation times, whereas in dry protein and polyglycine molecular reorientations could not be detected. The correlation time of the motion in the wet barstar at room temperature is 50-100 ms; the activation energy is about 80 kJ/mol. Previously, protein motions with such a long correlation time could be observed only by methods detecting chemical exchange in solution (e.g., hydrogen exchange). The application of solid-state MAS exchange spectroscopy provides new opportunities in studying slow biomolecular dynamics that is important for the biological function of proteins. 相似文献
104.
This study investigated the effects of different treatment of alkaline pH-shifting on milk protein concentrate (MPC), micellar casein concentrate (MCC) and whey protein isolate (WPI) assisted by the same ultrasound conditions, including changes in the physicochemical properties, solubility and foaming capacity. The solubility of milk proteins had a significant increase with gradual enhancement of ultrasound-assisted alkaline pH-shifting (p < 0.05), especially for MCC up to 99.50 %. Also, treatment made a significant decline in the particle size of MPC and MCC, as well as the turbidity of the proteins (p < 0.05). The foaming capacity of MPC, MCC, and WPI was all improved, especially at pH 11, and at this pH, the milk protein also showed the highest surface hydrophobicity. The best foaming capacity at pH 11 was the result of the combined effect of particle size, potential, protein conformation, solubility, and surface hydrophobicity. In conclusion, ultrasound-assisted pH-shifting treatment was found to be effective in improving the physicochemical properties and solubility and foaming capacity of milk proteins, especially MCC, with promising application prospect in food industry. 相似文献
105.
Preparation of pea protein isolate-xylan (PPI-X) conjugate-stabilized nanoemulsions using ultrasonic homogenization and the corresponding structure and environmental stability were investigated in this study. Conditions used to prepare nanoemulsions were optimized using a response surface methodology as follows: protein concentration 8.86 mg/mL, ultrasound amplitudes 57 % (370.5 W), and ultrasound time 16 min. PPI-X conjugate-stabilized nanoemulsions formed under these conditions exhibited less mean droplet size (189.4 ± 0.45 nm), more uniform droplet distribution, greater absolute value of zeta-potential (44.8 ± 0.22 mV), and higher protein adsorption content compared with PPI-stabilized nanoemulsions. PPI-X conjugate-stabilized nanoemulsions also exhibited even particle distribution and dense network structure, which might be reasons for the observed high interfacial protein adsorption content of conjugate-stabilized nanoemulsions. Moreover, better stability against environmental stresses, such as thermal treatment, freeze–thaw treatment, ionic strength and type, and storage time was also observed for the conjugate-stabilized nanoemulsions, indicating that this type of nanoemulsions possess a potential to endure harsh food processing conditions. Therefore, results provide a novel approach for the preparation of protein-polysaccharide conjugate-stabilized nanoemulsions to be applied as novel ingredients to meet special requirements of processed foods. 相似文献
106.
107.
Hardness and slip systems by an indentation method were investigated on different habit planes of orthorhombic hen egg-white lysozyme (O-HEWL) crystals containing water. A dependence of the hardness on the water-evaporation time exhibits three stages as incubation, transition and saturated ones, as tetragonal (T)-HEWL crystals reported previously. The hardness values of (1 1 0), (0 1 0) and (0 1 1) habit planes of O-HEWL in the incubation stage or wet condition exhibits 6, 8 and 10 MPa, respectively. The hardness depends on indented planes but it is independent of the air-humidity and crystal volumes. These values correspond to the intrinsic hardness for O-HEWL crystals containing water. In the incubation stage, the slip traces are clearly observed around the indentation mark and the corresponding six kinds of slip systems are identified to be {0 1 1}<1 0 0>, {1 1 0}<1 1 0>, {0 1 1}<0 1 1>, {1 1 0}<0 0 1>, {1 0 0}<0 0 1> and {0 1 0}<0 0 1>. 相似文献
108.
109.
110.
有序样品的固体核磁共振(NMR)已快速发展成测定蛋白质和多肽在“仿真”水化磷脂层中高分辨结构的重要谱学方法. 由于与膜相连的蛋白质和多肽的结构、动力学和功能往往都和其周边自然环境密切相关,因此人们把蛋白质和多肽有序排列于水化磷脂层中进行固体NMR测量, 从而获得与取向相关的各向异性自旋相互作用. 这些取向约束可作为结构参数重构蛋白质在水化磷脂层中的高分辨三维结构. 近十年来在样品制备,NMR探头和实验方法方面的显著发展,极大地促进了有序样品的固体NMR的发展,并使之成为测定与膜相连的蛋白质和多肽结构的有效方法. 该综述介绍有序样品的固体NMR谱学方法,并总结此领域里的最新研究进展. 相似文献