IRICA, Department of Inorganic, Organic and Biochemistry, Faculty of Chemical Sciences and Technologies, Universidad de Castilla-La Mancha (UCLM), Av. Camilo José Cela 10, 13071, Ciudad Real, Spain.
Laboratory of BioNanoTechnology, Wageningen University, 6700 EK, Wageningen, The Netherlands.
Nat Commun. 2023 Jun 30;14(1):3885. doi: 10.1038/s41467-023-39537-8.
Nuclear Magnetic Resonance (NMR) spectroscopy is a most powerful molecular characterization and quantification technique, yet two major persistent factors limit its more wide-spread applications: poor sensitivity, and intricate complex and expensive hardware required for sophisticated experiments. Here we show NMR with a single planar-spiral microcoil in an untuned circuit with hyperpolarization option and capability to execute complex experiments addressing simultaneously up to three different nuclides. A microfluidic NMR-chip in which the 25 nL detection volume can be efficiently illuminated with laser-diode light enhances the sensitivity by orders of magnitude via photochemically induced dynamic nuclear polarization (photo-CIDNP), allowing rapid detection of samples in the lower picomole range (normalized limit of detection at 600 MHz, nLOD, of 0.01 nmol Hz). The chip is equipped with a single planar microcoil operating in an untuned circuit that allows different Larmor frequencies to be addressed simultaneously, permitting advanced hetero-, di- and trinuclear, 1D and 2D NMR experiments. Here we show NMR chips with photo-CIDNP and broadband capabilities addressing two of the major limiting factors of NMR, by enhancing sensitivity as well as reducing cost and hardware complexity; the performance is compared to state-of-the-art instruments.
核磁共振(NMR)光谱学是一种非常强大的分子特征和定量技术,但有两个主要的持续因素限制了其更广泛的应用:灵敏度差,以及进行复杂实验所需的复杂、昂贵的硬件。在这里,我们展示了一种带有单平面螺旋微线圈的 NMR,该线圈位于未调谐电路中,具有极化选项,能够执行同时针对多达三种不同核素的复杂实验。一种微流控 NMR 芯片,其中 25 nL 的检测体积可以用激光二极管光有效地照射,通过光化学诱导动态核极化(photo-CIDNP)将灵敏度提高几个数量级,允许在低皮摩尔范围内快速检测样品(在 600 MHz 下的归一化检测限,nLOD,为 0.01 nmol Hz)。该芯片配备了一个单平面微线圈,在未调谐电路中运行,允许同时寻址不同的拉莫尔频率,从而实现高级异核、双核和三核、1D 和 2D NMR 实验。在这里,我们展示了具有 photo-CIDNP 和宽带功能的 NMR 芯片,通过提高灵敏度以及降低成本和硬件复杂性来解决 NMR 的两个主要限制因素;将性能与最先进的仪器进行了比较。