波谱学杂志 ›› 2015, Vol. 32 ›› Issue (1): 123-140.doi: 10.11938/cjmr20150114

• 综述评论 • 上一篇    

生物固体核磁共振中样品发热的研究进展

唐新启1,2,张正逢1,杨 俊1*   

  1. 1. 波谱与原子分子物理国家重点实验室,武汉磁共振中心(中国科学院 武汉物理与数学研究所),湖北 武汉 430071;
    2. 中国科学院大学,北京 100049
  • 收稿日期:2014-04-17 修回日期:2015-01-11 出版日期:2015-03-05 发布日期:2015-03-05
  • 作者简介:唐新启(1988-),男,湖北荆州人,硕士研究生,分析化学专业. *通讯联系人:杨俊,电话:027-87199723,E-mail:yangjun@wipm.ac.cn.
  • 基金资助:

    国家自然科学基金资助项目(21075133, 21173259).

Heating of Biological Samples in Studies of MAS Solid-State NMR

TANG Xin-qi1,2,ZHANG Zheng-feng1,YANG Jun1*   

  1. 1. State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Center for Magnetic Resonance(Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences), Wuhan 430071, China;
    2. University of Chinese Academy of Science, Beijing, 100049, China
  • Received:2014-04-17 Revised:2015-01-11 Online:2015-03-05 Published:2015-03-05
  • About author:*Corresponding author:YANG Jun, Tel: +86-27-87199723, E-mail: yangjun@wipm.ac.cn.
  • Supported by:

    国家自然科学基金资助项目(21075133, 21173259).

摘要:

近年来,固体核磁共振被广泛应用于膜蛋白、纤维化蛋白等体系的结构和功能研究.在固体核磁共振实验中,快速魔角旋转或高功率射频场照射等实验条件将导致样品发热.生物样品发热能导致严重的后果,例如样品温度的快速升高,信号分辨率、信噪比的降低,发热严重时甚至导致样品的不可逆损坏.近年来,人们对样品发热问题进行了一些研究,发现通过优化样品制备条件或固体核磁共振实验条件,以及改进探头设计等手段,可以在一定程度上减轻样品发热.该文主要综述了生物固体核磁共振研究中导致样品发热的原因和减轻样品发热的方法.

关键词: 固体核磁共振(solid-state NMR), 样品发热, 魔角旋转, 射频场

Abstract:

Magic-angle-spinning (MAS) solid-state NMR studies of biomolecules involve application of rapid sample rotation and radiofrequency pulsing, both of which can increase the sample temperature significantly, causing distorted spectra, sample dehydration and even sample degradation. In this review, the mechanisms leading to bio-sample heating in MAS solid-state NMR experiments are first introduced. The importance of sample temperature monitoring is then emphasized. Finally, we present the methods that can be used to to alleviate the problem, including optimization of sample preparation, selecting
optimal NMR parameters, and improving NMR spectrometer hardware such as the probes.

Key words: solid-state NMR, sample heating, magic angle spinning, radiofrequency

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