Malik Nikita, Kumar Ashutosh
Department of Bioscience and Bioengineering, Indian Institute of Technology Bombay, Powai, Mumbai, 400076, India.
J Biomol NMR. 2016 Sep;66(1):21-35. doi: 10.1007/s10858-016-0054-9. Epub 2016 Sep 1.
NMR resonance assignment of intrinsically disordered proteins poses a challenge because of the limited dispersion of amide proton chemical shifts. This becomes even more complex with the increase in the size of the system. Residue specific selective labeling/unlabeling experiments have been used to resolve the overlap, but require multiple sample preparations. Here, we demonstrate an assignment strategy requiring only a single sample of uniformly labeled (13)C,(15)N-protein. We have used a combinatorial approach, involving 3D-HNN, CC(CO)NH and 2D-MUSIC, which allowed us to assign a denatured centromeric protein Cse4 of 229 residues. Further, we show that even the less sensitive experiments, when used in an efficient manner can lead to the complete assignment of a complex system without the use of specialized probes in a relatively short time frame. The assignment of the amino acids discloses the presence of local structural propensities even in the denatured state accompanied by restricted motion in certain regions that provides insights into the early folding events of the protein.
由于酰胺质子化学位移的分散有限,对内在无序蛋白质进行核磁共振(NMR)共振归属具有挑战性。随着系统规模的增大,这一问题变得更加复杂。残基特异性选择性标记/未标记实验已被用于解决重叠问题,但需要进行多次样品制备。在此,我们展示了一种仅需一个均匀标记的(13)C、(15)N蛋白样品的归属策略。我们采用了一种组合方法,涉及3D-HNN、CC(CO)NH和2D-MUSIC,这使我们能够对229个残基的变性着丝粒蛋白Cse4进行归属。此外,我们表明,即使是灵敏度较低的实验,若能以高效方式使用,也可在相对较短的时间内,在不使用专门探针的情况下实现对复杂系统的完全归属。氨基酸的归属揭示了即使在变性状态下局部结构倾向的存在,同时某些区域存在受限运动,这为蛋白质的早期折叠事件提供了见解。