Iali Wissam, Moustafa Gamal A I, Dagys Laurynas, Roy Soumya S
Department of Chemistry, King Fahd University of Petroleum and Minerals (KFUPM), Dhahran, Saudi Arabia.
Department of Medicinal Chemistry, Faculty of Pharmacy, Minia University, Minia, Egypt.
Magn Reson Chem. 2021 Dec;59(12):1199-1207. doi: 10.1002/mrc.5144. Epub 2021 Mar 8.
Signal amplification by reversible exchange (SABRE) offers a cost-effective route to boost nuclear magnetic resonance (NMR) signal by several orders of magnitude by employing readily available para-hydrogen as a source of hyperpolarisation. Although H spins have been the natural choice of SABRE hyperpolarisation since its inception due to its simplicity and accessibility, limited spin lifetimes of H makes it harder to employ them in a range of time-dependent NMR experiments. Heteronuclear spins, for example, C and N, in general have much longer T lifetimes and thereby are found to be more suitable for hyperpolarised biological applications as demonstrated previously by para-hydrogen induced polarisation (PHIP) and dynamic nuclear polarisation (DNP). In this study we demonstrate a simple procedure to enhance N signal of an antibiotic drug ornidazole by up to 71,000-folds with net N polarisation reaching ~23%. Further, the effect of co-ligand strategy is studied in conjunction with the optimum field transfer protocols and consequently achieving N hyperpolarised spin lifetime of >3 min at low field. Finally, we present a convenient route to harness the hyperpolarised solution in aqueous medium free from catalyst contamination leading to a strong N signal detection for an extended duration of time.
通过可逆交换进行信号放大(SABRE)提供了一种经济高效的途径,通过使用 readily available 的仲氢作为超极化源,将核磁共振(NMR)信号提高几个数量级。尽管自 SABRE 超极化技术诞生以来,由于其简单性和可及性,H 自旋一直是其自然选择,但 H 自旋的有限自旋寿命使得在一系列与时间相关的 NMR 实验中使用它们变得更加困难。例如,异核自旋 C 和 N,通常具有长得多的 T 寿命,因此如先前通过仲氢诱导极化(PHIP)和动态核极化(DNP)所证明的,它们被发现更适合用于超极化生物应用。在本研究中,我们展示了一种简单的方法,可将抗生素药物奥硝唑的 N 信号增强高达 71,000 倍,净 N 极化达到约 23%。此外,结合最佳场转移协议研究了共配体策略的效果,从而在低场下实现了大于 3 分钟的 N 超极化自旋寿命。最后,我们提出了一种便捷的途径,在无催化剂污染的水性介质中利用超极化溶液,从而在延长的时间内实现强 N 信号检测。