¹⁹F magic angle spinning (MAS) NMR spectroscopy is a powerful tool for characterization of fluorinated solids. The recent development of ¹⁹F MAS NMR probes, operating at spinning frequencies of 60–111 kHz, enabled analysis of systems spanning from organic molecules to pharmaceutical formulations to biological assemblies, with unprecedented resolution. Herein, we systematically evaluate the benefits of high MAS frequencies (60–111 kHz) for 1D and 2D ¹⁹F-detected experiments in two pharmaceuticals, the antimalarial drug mefloquine and a formulation of the cholesterol-lowering drug atorvastatin calcium. We demonstrate that ¹H decoupling is essential and that scalar-based, heteronuclear single quantum coherence (HSQC) and heteronuclear multiple quantum coherence (HMQC) correlation experiments become feasible and efficient at the MAS frequency of 100 kHz. This study opens doors for the applications of high frequency ¹⁹F MAS NMR to a wide range of problems in chemistry and biology.

¹⁹ F 魔角旋转 (MAS) NMR 光谱是表征氟化固体的强大工具。最近开发的¹⁹ F MAS NMR 探头在 60-111 kHz 的旋转频率下运行，能够以前所未有的分辨率分析从有机分子到药物配方再到生物组装体的系统。在此，我们系统地评估了高 MAS 频率 (60–111 kHz)对于两种药物（抗疟药甲氟喹和降胆固醇药物阿托伐他汀钙制剂）的1D 和 2D ¹⁹ F 检测实验的益处。我们证明¹H 解耦至关重要，基于标量的异核单量子相干 (HSQC) 和异核多量子相干 (HMQC) 相关实验在 100 kHz 的 MAS 频率下变得可行且高效。这项研究为高频¹⁹ F MAS NMR 应用到化学和生物学领域的广泛问题打开了大门。