Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR
Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR
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DOI：
10.1016/j.jmr.2015.08.003
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发表时间：
2015-10-01
影响因子：
2.2
通讯作者：
Fujiwara, Toshimichi
中科院分区：
文献类型：
--
作者：
Matsuki, Yoh;Nakamura, Shinji;Fujiwara, Toshimichi
魔角自旋（MAS）NMR是研究分子结构和动力学的有力工具，但其灵敏度低。在这里，我们开发了一种新的氦冷却MAS NMR探头系统，采用闭环气体再循环机制。除了由于低温引起的灵敏度增益之外，本系统还能够在低温温度（T= 35-120 K）下实现高度稳定的MAS（v（R）= 4-12 kHz）超过一周，而不消耗氦气，电力成本为16 kW/h。在T=40 K和B-0 = 16.4 T下记录结晶三肽样品的高分辨率1D和2D数据，其中证明了相对于室温测量的灵敏度增益的数量级。低成本和长期稳定的MAS有力地促进了蛮力灵敏度增强多维MAS NMR以及在低于100 K的温度范围内的动态核极化（DNP）增强NMR的更广泛应用。(C)2015年，作者。爱思唯尔公司出版
Magic-angle spinning (MAS) NMR is a powerful tool for studying molecular structure and dynamics, but suffers from its low sensitivity. Here, we developed a novel helium-cooling MAS NMR probe system adopting a closed-loop gas recirculation mechanism. In addition to the sensitivity gain due to low temperature, the present system has enabled highly stable MAS (v(R) = 4-12 kHz) at cryogenic temperatures (T= 35-120 K) for over a week without consuming helium at a cost for electricity of 16 kW/h. High-resolution 1D and 2D data were recorded for a crystalline tri-peptide sample at T=40 K and B-0 = 16.4 T, where an order of magnitude of sensitivity gain was demonstrated versus room temperature measurement. The low-cost and long-term stable MAS strongly promotes broader application of the brute-force sensitivity-enhanced multi-dimensional MAS NMR, as well as dynamic nuclear polarization (DNP)-enhanced NMR in a temperature range lower than 100 K. (C) 2015 The Authors. Published by Elsevier Inc.