Simultaneous Multi-Slice Selective Constant-Time J-Resolved Spectroscopy for Measuring J Values

doi:10.11938/cjmr20192775

Abstract

Abstract: Scalar coupling is an important parameter in nuclear magnetic resonance (NMR). The proton-proton coupling constant J_H-H provides valuable information on molecular structure. However, determining J_H-H value in complex coupling networks is still challenging. Here, we propose a method called simultaneous multi-slice selective constant-time J-resolved spectroscopy (SMS-SECTJRES) to measure J_H-H values of all coupling networks of a molecule simultaneously in one experiment. In this method, gradient-encoded selective refocusing is used during a fixed evolution time, combined with echo planar spectroscopic imaging (EPSI) detection module to extract different selective J-edited spectra in different spatial positions. This new method is conducive to reveal coupling networks and the analysis of molecular structures.

Key words: nuclear magnetic resonance (NMR), scalar coupling, selective constant-time, echo planar spectroscopic imaging (EPSI), molecular structure elucidation

CLC Number:

O482.53

CHEN Jin-yong, ZENG Qing, LIN Yan-qin, CHEN Zhong. Simultaneous Multi-Slice Selective Constant-Time J-Resolved Spectroscopy for Measuring J Values[J]. Chinese Journal of Magnetic Resonance, 2019, 36(4): 456-462.

References

[1] DONG J Y, XU L, CAO H T, et al. A new data processing method for metabonomic and its application in a study of diabetes[J]. Chinese J Magn Reson, 2007, 24(4):381-393. 董继扬, 徐乐, 曹红婷, 等. 代谢组学数据分析方法及在糖尿病研究中的应用[J]. 波谱学杂志, 2007, 24(4):381-393.
[2] ZHANG F, LIN D H. Interaction of proteins with metal ions studied by NMR techniques:A review[J]. Chinese J Magn Reson, 2009, 26(1):136-149. 张芳, 林东海. 用核磁共振方法研究金属离子与蛋白质的相互作用[J]. 波谱学杂志, 2009, 26(1):136-149.
[3] CHAI X, SUN P, YUAN B, et al. Fast detection of choline containing compounds in dairy products using NMR[J]. Chinese J Magn Reson, 2018, 35(2):178-187. 柴鑫, 孙鹏, 袁斌, 等. 乳制品中胆碱及其衍生物的快速核磁共振检测[J]. 波谱学杂志, 2018, 35(2):178-187.
[4] ZHOU Z M, LIU M L, ZHANG X, et al. Two effective methods for improving NMR sensitivity and resolution in studies of biomacromolecules:TROSY and CRINEPT[J]. Chinese J Magn Reson, 2004, 21(3):371-383. 周志明, 刘买利, 张许, 等. 提高生物大分子NMR分辨率和灵敏度的有效方法:TROSY和CRINEPT[J]. 波谱学杂志, 2004, 21(3):371-383.
[5] SUN Y, CHEN Y K, LI J P, et al. Efficiency of double cross polarization in magic-angle spinning solid-state nmr studies on membrane proteins[J]. Chinese J Magn Reson, 2017, 34(3):257-265. 孙毅, 陈艳可, 李建平, 等. 固体核磁共振中膜蛋白双交叉极化效率与动力学参数相关的定量分析[J]. 波谱学杂志, 2017, 34(3):257-265.
[6] LIN Y Q, ZENG Q, LIN L J, et al. High-resolution methods for the measurement of scalar coupling constants[J]. Prog Nucl Magn Reson Spectrosc, 2018, 109:135-159.
[7] FACKE T, SERF B S. A new method for H,H spin-coupling measurement in organic chemistry[J]. J Magn Reson, 1995, 113(1):114-116.
[8] GIRAUD N, BEGUIN L, COURTIEU J, et al. Nuclear magnetic resonance using a spatial frequency encoding:application to J-edited spectroscopy along the sample[J]. Angew Chem Int Ed Engl, 2010, 49(20):3481-3484.
[9] SINNAEVE D, FOROOZANDEH M, NILSSON M, et al. A general method for extracting individual coupling constants from crowded ¹H NMR spectra[J]. Angew Chem Int Ed Engl, 2016, 55:1090-1093.
[10] LIN L J, WEI Z L, LIN Y Q, et al. Measuring JH-H values with a selective constant-time 2D NMR protocol[J]. J Magn Reson, 2016, 272:20-24.
[11] ZENG Q, LIN L J, CHEN J Y, et al. A simultaneous multi-slice selective J-resolved experiment for fully resolved scalar coupling information[J]. J Magn Reson, 2017, 282:27-31.
[12] ZANGGER K, STERK H. Homonuclear broadband-decoupled NMR spectra[J]. J Magn Reson, 1997, 124:486-489.
[13] FOROOZANDEH M, ADAMS R W, MEHARRY N J, et al. Ultrahigh-resolution NMR spectroscopy[J]. Angew Chem Int Ed Engl, 2014, 53(27):6990-6992.

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