JEOL Ltd, 3-1-2 Musashino, Akishima, Tokyo 196-8558, Japan.
J Magn Reson. 2011 Jan;208(1):44-8. doi: 10.1016/j.jmr.2010.10.001. Epub 2010 Oct 8.
Substantial resolution and sensitivity enhancements of solid-state (1)H detected (14)N HMQC NMR spectra at very fast MAS rates up to 80 kHz, in a 1mm MAS rotor, are presented. Very fast MAS enhances the (1)H transverse relaxation time and efficiently decouples the (1)H-(14)N interactions, both effects leading to resolution enhancement. The micro-coil contributes to the sensitivity increase via strong (14)N rf fields and high sensitivity per unit volume. (1)H-(14)N HMQC 2D spectra of glycine and glycyl-L-alanine at 70 kHz MAS at 11.7 T are observed in a few minutes with a sample volume of 0.8 μL.
本文介绍了在 1mm 转子中，高达 80kHz 的非常快的 MAS 速率下，固态（1）H 检测（14）N HMQC NMR 谱的大幅度分辨率和灵敏度增强。非常快的 MAS 增强了（1）H 横向弛豫时间，并有效地解耦了（1）H-（14）N 相互作用，这两种效应都导致了分辨率的提高。微线圈通过强（14）N rf 场和单位体积的高灵敏度有助于提高灵敏度。在 11.7T 下，70kHz MAS 时，仅用 0.8μL 的样品体积，就可以在几分钟内观察到甘氨酸和甘氨酰-L-丙氨酸的（1）H-（14）N HMQC 2D 谱。
