Laszlo Kenneth J, Munger Eleanor B, Bush Matthew F
Department of Chemistry, University of Washington , Box 351700, Seattle, Washington 98195-1700, United States.
J Phys Chem B. 2017 Apr 6;121(13):2759-2766. doi: 10.1021/acs.jpcb.7b00783. Epub 2017 Mar 24.
The fidelity between the structures of proteins in solution and protein ions in the gas phase is critical to experiments that use gas-phase measurements to infer structures in solution. Here we generate ions of lysozyme, a 129-residue protein whose native tertiary structure contains four internal disulfide bonds, from three solutions that preserve varying extents of the original native structure. We then use cation-to-anion proton-transfer reactions (CAPTR) to reduce the charge states of those ions in the gas phase and ion mobility to probe their structures. The collision cross section (Ω) distributions of each CAPTR product depends to varying extents on the original solution, the charge state of the product, and the charge state of the precursor. For example, the Ω distributions of the 6+ ions depend strongly on the original solutions conditions and to a lesser extent on the charge state of the precursor. Energy-dependent experiments suggest that very different structures are accessible to disulfide-reduced and disulfide-intact ions, but similar Ω distributions are formed at high energy for disulfide-intact ions from denaturing and from aqueous conditions. The Ω distributions of the 3+ ions are all similar but exhibit subtle differences that depend more strongly on the original solutions conditions than other factors. More generally, these results suggest that specific CAPTR products may be especially sensitive to specific elements of structure in solution.
溶液中蛋白质结构与气相中蛋白质离子结构之间的保真度对于利用气相测量推断溶液中结构的实验至关重要。在此,我们从三种不同程度保留原始天然结构的溶液中生成了溶菌酶离子,溶菌酶是一种含有129个残基的蛋白质,其天然三级结构包含四个内部二硫键。然后,我们使用阳离子到阴离子的质子转移反应(CAPTR)在气相中降低这些离子的电荷态,并利用离子迁移率来探测它们的结构。每个CAPTR产物的碰撞截面(Ω)分布在不同程度上取决于原始溶液、产物的电荷态以及前体的电荷态。例如,6+离子的Ω分布强烈依赖于原始溶液条件,而对前体电荷态的依赖程度较小。能量相关实验表明,二硫键还原和二硫键完整的离子可形成非常不同的结构,但对于来自变性条件和水性条件的二硫键完整离子,在高能下会形成相似的Ω分布。3+离子的Ω分布都相似,但表现出细微差异,这些差异比其他因素更强烈地依赖于原始溶液条件。更普遍地说,这些结果表明特定的CAPTR产物可能对溶液中特定的结构元素特别敏感。