Sensitivity enhancement of multidimensional NMR experiments by paramagnetic relaxation effects

Sensitivity enhancement of multidimensional NMR experiments by paramagnetic relaxation effects
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DOI:
10.1021/ja0634526
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发表时间:
2006-10-18
影响因子:
15
通讯作者:
Chen, Yuan
Chen, Yuan
中科院分区:
化学1区
文献类型:
--
作者:
Cai, Sheng;Seu, Candace;Chen, Yuan

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开发核磁共振方法的主要目标之一是提高多维核磁共振实验的灵敏度或减少所需的采集时间。在这些实验中,核磁共振仪器80%以上的时间都花在了循环延迟上,仪器在那里闲置,等待质子磁化的恢复。在这项研究中,我们报告了一种利用顺磁驰豫效应来缩短生物大分子多维核磁共振实验中所需的循环延迟的方法。这种方法大大减少了核磁共振仪器所需的时间。Ni2+离子与螯合分子DO2A络合后,可缩短生物大分子的质子T-1弛豫时间,而不会产生大多数顺磁性离子所具有的显著谱线展宽效应。Ni(DO2A)还显著缩短了水的T-1弛豫时间,从而通过消除不稳定的酰胺共振的饱和而提供了额外的灵敏度增益。
One of the main goals of NMR method development is to increase the sensitivity of multidimensional NMR experiments or reduce the required acquisition time. In these experiments, more than 80% of the NMR instrument time is spent on the recycle delay, where the instrument idles to wait for the recovery of proton magnetization. In this study, we report a method of using paramagnetic relaxation effects to shorten the recycle delays required in multidimensional NMR experiments of biological macromolecules. This approach significantly reduces the NMR instrument time required. Ni2+ ion, complexed with the chelating molecule DO2A, is used to decrease the proton T-1 relaxation time of biological macromolecules without the significant line-broadening effects that are associated with most paramagnetic ions. The Ni(DO2A) also significantly decreases the T-1 relaxation time of water, thus providing additional sensitivity gain by eliminating the saturation of labile amide resonances.