Abstract

While many drugs and metabolites contain nitrogen, harnessing their diagnostic 15N 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 d9-benzylamine allows the naturally abundant 15N NMR signatures of pyridine, pyrazine, metronidazole, and acetonitrile to be readily detected at 9.4 T in single NMR observations through >50% 15N polarization levels. These signals allow for rapid and precise reagent quantification via a response that varies linearly over the 2–70 mM concentration range.

Highlights

  • Hyperpolarization methods have been shown to dramatically improve the sensitivity of nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI)[1,2] in a process that involves increasing the purity of the magnetic states they detect

  • We start by considering nonlabeled pyridine at 35 mM concentration because of its wide use in early Signal amplification by reversible exchange (SABRE) research[3,4,13] in conjunction with the precatalyst [IrCl(COD)(h22-1)]43 (5 mM) of Scheme 1

  • Our experimental measurements involved examining an NMR tube containing methanold[4] solutions of these reagents under 3 bar pressure of p-H2 at 99% purity. p-H2 gas is first dissolved by shaking the NMR tube while it is located in a preset magnetic field that lies between ±1 mG and ±70 G for ∼10 s

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Summary

Introduction

Hyperpolarization methods have been shown to dramatically improve the sensitivity of nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI)[1,2] in a process that involves increasing the purity of the magnetic states they detect. The SABRE catalyst [Ir(H)2(h221)(py)3]Cl forms and a 1H NMR signal gain of 1452-fold can be seen for the ortho proton resonance of free pyridine that is present in the solution after being transferred from a 60 G field.

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