Deuteron-proton isotope correlation spectroscopy at high magnetic fields

IF 1.8 3区化学 Q4 CHEMISTRY, PHYSICAL

Solid state nuclear magnetic resonance Pub Date : 2025-02-04 DOI:10.1016/j.ssnmr.2025.101993

Neethu Thomas , Claire Welton , Tomasz Pawlak , Parth Raval , Julien Trébosc , Sheetal K. Jain , G.N. Manjunatha Reddy

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引用次数: 0

Abstract

A cross-polarization ²H–¹H isotope correlation spectroscopy (CP-iCOSY) approach is presented for characterizing a deuterated amino acid, pharmaceutical compound and a solid formulation. This can be achieved by isotopic enrichment in conjunction with high magnetic field (28.2 T) and fast magic-angle spinning (MAS), enabling the rapid detection of ²H NMR spectra in a few seconds to minutes. Specifically, two-dimensional (2D) ²H–¹H CP-iCOSY experiment allows the local structures and through-space interactions in a partially deuterated compounds to be elucidated. In doing so, we compare conventional spin-lock and rotor-echo-short-pulse-irradiation ^RESPIRATIONCP sequences for acquiring 2D ¹H–²H correlation spectra. The ^RESPIRATIONCP sequence allows the detection of 2D peaks at lower CP contact times (0.1–1 ms) than the conventional CP (0.2–4 ms) sequence. Analysis of partially deuterated L-histidine·HCl·H₂O and dopamine.HCl is presented, in which the detection of 2D peaks corresponding to ²H–¹H pairs separated by greater than 4 Å distance demonstrates the potential of the presented approach for the characterization of packing interactions. These results are corroborated by NMR crystallography analysis using the Gauge-Including Projector Augmented-Wave (GIPAW) approach.

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来源期刊

Solid state nuclear magnetic resonance 物理-光谱学

CiteScore

5.30

自引率

9.40%

发文量

审稿时长

72 days

期刊介绍： The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.