Zhou Donghua H, Rienstra Chad M
Department of Chemistry, University of Illinois at Urbana-Champaign, Urbana, IL 61801, USA.
J Magn Reson. 2008 May;192(1):167-72. doi: 10.1016/j.jmr.2008.01.012. Epub 2008 Feb 1.
High-sensitivity proton detected experiments in solid-state NMR have been recently demonstrated in proton diluted proteins as well as fully protonated samples under fast magic-angle spinning. One key element for performing successful proton detection is effective solvent suppression achieved by pulsed field gradients (PFG) and/or saturation pulses. Here we report a high-performance solvent suppression method that attenuates multiple solvent signals simultaneously by more than a factor of 10,000, achieved by an optimized combination of homospoil gradients and supercycled saturation pulses. This method, which we call Multiple Intense Solvent Suppression Intended for Sensitive Spectroscopic Investigation of Protonated Proteins, Instantly (MISSISSIPPI), can be applied without a PFG probe. It opens up new opportunities for two-dimensional heteronuclear correlation spectroscopy of hydrated proteins at natural abundance as well as high-sensitivity and multi-dimensional experimental investigation of protein-solvent interactions.
最近,在快速魔角旋转条件下,高灵敏度质子检测实验已在质子稀释蛋白以及完全质子化样品的固态核磁共振中得到证实。成功进行质子检测的一个关键要素是通过脉冲场梯度(PFG)和/或饱和脉冲实现有效的溶剂抑制。在此,我们报告一种高性能溶剂抑制方法,该方法通过同相破坏梯度和超循环饱和脉冲的优化组合,能同时将多个溶剂信号衰减至10000倍以上。我们将此方法称为用于质子化蛋白质敏感光谱研究的即时多重强溶剂抑制(MISSISSIPPI),它无需PFG探头即可应用。这为天然丰度下的水合蛋白二维异核相关光谱以及蛋白质 - 溶剂相互作用的高灵敏度和多维实验研究开辟了新机遇。