Remarkable Levels of 15N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level
Remarkable Levels of 15N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level
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DOI：
10.1021/acs.jpcb.0c02583
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发表时间：
2020-06-04
影响因子：
3.3
通讯作者：
Duckett, Simon B.
中科院分区：
文献类型：
--
作者：
Fekete, Marianna;Ahwal, Fadi;Duckett, Simon B.
虽然许多药物和代谢物含有氮，但由于固有的检测困难，利用其诊断性N-15 NMR特征进行表征尚未得到充分利用。在这里，我们演示了如何通过可逆交换精确的超低场信号放大（+/-0.2mG）结合仲氢和IrCl（COD）-（NHC）形式的铱预催化剂与共配体d（9）-苄胺，允许吡啶、吡嗪、甲硝唑、和乙腈在9.4 T下通过> 50%N-15极化水平在单次NMR观察中容易检测。这些信号允许通过在2 - 70 mM浓度范围内线性变化的响应进行快速和精确的试剂定量。
While many drugs and metabolites contain nitrogen, harnessing their diagnostic N-15 NMR signature for their characterization is underutilized because of inherent detection difficulties. Here, we demonstrate how precise ultralow field signal amplification by reversible exchange (+/- 0.2 mG) in conjunction parahydrogen and an iridium precatalyst of the form IrCl(COD)-(NHC) with the coligand d(9)-benzylamine allows the naturally abundant N-15 NMR signatures of pyridine, pyrazine, metronidazole, and acetonitrile to be readily detected at 9.4 T in single NMR observations through >50% N-15 polarization levels. These signals allow for rapid and precise reagent quantification via a response that varies linearly over the 2-70 mM concentration range.