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Sensitivity-enhanced detection of non-labile proton and carbon NMR spectra on water resonances

机译：在水共振上增强了非不稳定质子和碳NMR光谱的敏感性增强

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摘要

Chemical exchange saturation transfer (CEST) experiments enhance the NMR signals of labile protons by continuously transferring these protons' saturation to an abundant solvent pool like water. The present study expands these principles by fusing into these experiments homonuclear isotropic mixing sequences, enabling the water-enhanced detection of non-exchangeable species. Further opportunities are opened by the addition of coupling-mediated heteronuclear polarization transfers, which then impose on the water resonance a saturation stemming from non-labile heteronuclear species like C-13. To multiplex the ensuing experiments, these relayed approaches are combined with time-domain schemes involving multiple Ramsey-labeling experiments imparting the frequencies of the non-labile sites on the water resonance, via chemical exchange. C-13 and H-1 NMR spectra were detected in this fashion with about two-fold SNR amplification vis-a-vis conventionally detected spectroscopies. When combined with nonuniform sampling principles, this methodology thus becomes a sensitive alternative to detect nonexchangeable species in biomolecules. Still, multiple parameters including the scalar couplings and solvent exchange rates, will affect the efficiency and consequently the practicality of the overall experiment.
机译：化学交换饱和度转移（CEST）实验通过连续将这些质子饱和度连续地将这些质子的饱和度饱和至像水等丰富的溶剂池中增强了不稳定质子的NMR信号。本研究通过融合到这些实验同核各向同性混合序列，使得能量增强的不可交换物种检测来扩展这些原理。通过加入偶联介导的异核偏振转移，将进一步的机会打开，然后施加水共振来自非不稳定的异核物种如C-13的饱和度。为了复用随后的实验，这些中继方法与涉及多个Ramsey标记实验的时域方案，通过化学交换赋予水共振上的非不稳定部位的频率。以这种方式检测C-13和H-1 NMR光谱，其具有约两倍的SNR扩增Vis-A-VI常规检测到的光谱谱。当与非均匀采样原理结合时，该方法因此成为检测生物分子中非掺杂物种的敏感替代物。尽管如此，包括标量耦合和溶剂汇率的多个参数会影响效率，从而影响整体实验的实用性。

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