An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes

Abstract

To optimize sensitivity, there has been an increasing interest in the miniaturization of NMR detectors. In our lab, a stripline NMR detector has been developed, which provides high resolution and is scalable to a large range of sample volumes. These features make it an ideal detector for hyphenated techniques. In this manuscript, we demonstrate a stripline probe, which is designed for combining supercritical fluid chromatography (SFC) experiments with NMR. It features a novel stripline chip, designed to reduce the signal from the contact pads, which results in an improved lineshape. An external lock circuit provides stability over time to perform signal averaging or multidimensional experiments. As proof of concept, we demonstrate the SFC-NMR technique with this stripline probe using a mixture of cholesterol and cholestanol, which is relevant for studying cerebrotendinous xanthomatosis. Additionally, this probe makes it possible to record high-resolution spectra of samples with a high spin density. This means that it is possible to directly observe shifts due to the nuclear demagnetizing field in the “homomolecular” case, which is challenging using conventional probes due to broadening effects from radiation damping.