NOE analysis using dual injection DNP-NMR for studies of solvent–solute interactions at low concentrations

IF 1.7 4区 化学 Bulletin of the Korean Chemical Society Pub Date : 2024-05-09 DOI:10.1002/bkcs.12852
Jihyun Kim
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Abstract

Dynamic nuclear polarization (DNP) offers significant signal enhancement compared to conventional nuclear magnetic resonance (NMR) in measuring the nuclear Overhauser effect. Owing to this enhancement, DNP enables the quantitative analysis of solvent–solute interactions, which are typically challenging to assess using standard NMR techniques. However, current experimental setups generally require the use of samples with relatively high solute concentrations because of large dilution factors. This limits the studies on solvent–solute interactions for bio-related molecules, particularly those with low solubility. In such cases, the concentration of solute post-dilution often falls below the detection limits. Herein, we introduce a novel dual injection system designed to considerably increase the dilution factor, thereby enabling the use of samples with lower solute concentrations while maintaining detectable signal levels. The effectiveness of this system was demonstrated in experiments using trifluoroacetic acid at concentrations 50 times lower than those used in the conventional method.

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利用双注入 DNP-NMR 进行 NOE 分析,研究低浓度溶剂与溶质之间的相互作用
与传统的核磁共振(NMR)相比,动态核偏振(DNP)在测量核奥弗霍塞尔效应时能显著增强信号。由于这种增强作用,DNP 能够对溶剂-溶质相互作用进行定量分析,而使用标准 NMR 技术通常很难对这种相互作用进行评估。然而,由于稀释因子较大,目前的实验装置通常需要使用溶质浓度相对较高的样品。这就限制了对生物相关分子,尤其是低溶解度分子的溶剂-溶质相互作用的研究。在这种情况下,稀释后的溶质浓度往往低于检测限。在此,我们介绍了一种新型的双进样系统,其设计可显著提高稀释因子,从而在使用溶质浓度较低的样品时也能保持可检测的信号水平。在使用浓度比传统方法低 50 倍的三氟乙酸进行的实验中,证明了该系统的有效性。
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来源期刊
Bulletin of the Korean Chemical Society
Bulletin of the Korean Chemical Society Chemistry-General Chemistry
自引率
23.50%
发文量
182
期刊介绍: The Bulletin of the Korean Chemical Society is an official research journal of the Korean Chemical Society. It was founded in 1980 and reaches out to the chemical community worldwide. It is strictly peer-reviewed and welcomes Accounts, Communications, Articles, and Notes written in English. The scope of the journal covers all major areas of chemistry: analytical chemistry, electrochemistry, industrial chemistry, inorganic chemistry, life-science chemistry, macromolecular chemistry, organic synthesis, non-synthetic organic chemistry, physical chemistry, and materials chemistry.
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