Ultra-selective 1D clean in-phase correlation spectroscopy

Taylor, Daniel Aaron; Király, Péter; Bowyer, Paul; Nilsson, Mathias; Castañar, Laura; Morris, Gareth A.; Adams, Ralph W.

doi:10.1039/d3cc01333b

Cited by 9 publications

(5 citation statements)

References 34 publications

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“…Such sequences have further potential application in multidimensional pure shift experiments, such as TOCSY-PSYCHE, which would enable acquisition of ultrahigh-resolution correlation experiments in nondeuterated solvents. Furthermore, as PSYCHE-iWG provides chemical shift information for each multiplet, ultraselective 1D correlation NMR experiments (such as the GEMSTONE family of experiments) − can be used as fast alternatives to 2D experiments for characterization.…”

Section: Discussionmentioning

confidence: 99%

Solvent Suppression in Pure Shift NMR

Gates,

Bradley,

Berry

et al. 2024

Anal. Chem.

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Intense solvent signals in 1 H solution-state NMR experiments typically cause severe distortion of spectra and mask nearby solute signals. It is often infeasible or undesirable to replace a solvent with its perdeuterated form, for example, when analyzing formulations in situ, when exchangeable protons are present, or for practical reasons. Solvent signal suppression techniques are therefore required. WATERGATE methods are well-known to provide good solvent suppression while enabling retention of signals undergoing chemical exchange with the solvent signal. Spectra of mixtures, such as pharmaceutical formulations, are often complicated by signal overlap, high dynamic range, the narrow spectral width of 1 H NMR, and signal multiplicity. Here, we show that by combining WATERGATE solvent suppression with pure shift NMR, ultrahigh-resolution 1 H NMR spectra can be acquired while suppressing intense solvent signals and retaining exchangeable 1 H signals. The new method is demonstrated in the analysis of cyanocobalamin, a vitamin B12 supplement, and of an eye-drop formulation of atropine.

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Section: Discussionmentioning

confidence: 99%

Solvent Suppression in Pure Shift NMR

Gates,

Bradley,

Berry

et al. 2024

Anal. Chem.

Self Cite

View full text Add to dashboard Cite

show abstract

“…Such sequences have further potential application in multidimensional pure shift experiments, such as TOCSY-PSYCHE, 32 which would enable acquisition of ultrahigh resolution correlation experiments in non-deuterated solvents. Furthermore, as PSYCHE-iWG provides chemical shift information for each multiplet, ultraselective 1D correlation NMR experiments (such as the GEMSTONE family of experiments) [33][34][35][36] can be used as fast alternatives to 2D experiments for characterization.…”

Section: Discussionmentioning

confidence: 99%

Solvent suppression in pure shift NMR

Gates,

Bradley,

Berry

et al. 2023

Preprint

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Intense solvent signals in 1H solution state NMR experiments typically cause severe distortion of spectra and mask nearby solute signals. It is often infeasible or undesirable to replace a solvent with its perdeuteriated form, for example when analysing formulations in situ, when exchangeable protons are present, or for practical reasons. Solvent signal suppression techniques are therefore required. WATERGATE methods are well known to provide good solvent suppression while enabling retention of signals undergoing chemical exchange with the solvent signal. Spectra of mixtures, such as pharmaceutical formulations, are often complicated by signal overlap, high dynamic range, the narrow spectral width of 1H NMR, and signal multiplicity. Here, we show that, by combining WATERGATE solvent suppression with pure shift NMR, ultra-high resolution 1H NMR spectra can be acquired while suppressing intense solvent signals and retaining exchangeable 1H signals. The new method is demonstrated in the analysis of cyanocobalamin, a vitamin B12 supplement, and an eye-drop formulation of atropine.

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“…Notably, benefiting from single-scan ultrahigh-selective excitation of targeted resonances, the recent GEMSTONE method 18 applications, including GEMSTONE-NOESY, 18 GEM-STONE-TOCSY, 19 GEMSTONE-ROESY, 20 and in-phase GEMSTONE-COSY. 21 As one of the CSSF-TOCSY methods that introduce the CSSF techniques into selective TOCSY experiments, a hybrid of the GEMSTONE and selective TOCSY 19 enables the extraction of totally correlated 1D spectra associated with the peaks of interest in overlapped multiplets within a single scan, thus facilitating mixture analysis and molecular structure determination. Nevertheless, in cases involving probing complex sample systems, subspectra containing complete coupling information on targeted resonances remain confined by the crowded resonances.…”

Section: ■ Introductionmentioning

confidence: 99%

Combining Fast Pure Shift NMR and GEMSTONE-Based Selective TOCSY for Efficient NMR Analysis of Complex Systems

Zhan,

Liu,

Fang

et al. 2024

Anal. Chem.

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As one of the commonly used intact detection techniques, liquid NMR spectroscopy offers unparalleled insights into the chemical environments, structures, and dynamics of molecules. However, it generally encounters the challenges of crowded or even overlapped spectra, especially when probing complex sample systems containing numerous components and complicated molecular structures. Herein, we exploit a general NMR protocol for efficient NMR analysis of complex systems by combining fast pure shift NMR and GEMSTONE-based selective TOCSY. First, this protocol enables ultrahigh-selective observation on the coupling networks that are totally correlated with targeted resonances or components, even where they are situated in severely overlapped spectral regions. Second, pure shift simplification is introduced to enhance the spectral resolution and further resolve the subspectra containing spectral congestion, thus facilitating the dissection of overlapped spectra. Additionally, sparse sampling accompanied by spectral reconstruction is adopted to significantly accelerate acquisition and improve spectral quality. The advantages of this protocol were demonstrated on different complex sample systems, including a challenging compound of estradiol, a mixture of sucrose and D-glucose, and natural grape juice, verifying its feasibility and power, and boosting the potential application landscapes in various chemical fields.

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Ultra-selective 1D clean in-phase correlation spectroscopy

Abstract: Selective 1D COSY can unambiguously identify coupled spins but is often limited both by lack of selectivity, and by unfavourable multiplet lineshapes. Here, ultra selective GEMSTONE excitation is employed with...

Cited by 9 publications

References 34 publications

Solvent Suppression in Pure Shift NMR

Solvent Suppression in Pure Shift NMR

Solvent suppression in pure shift NMR

Combining Fast Pure Shift NMR and GEMSTONE-Based Selective TOCSY for Efficient NMR Analysis of Complex Systems

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