600 MHz NMR spectrometer

600MHz核磁共振波谱仪

• 批准号: 521411486
• 金额: --
• 依托单位: Technische Universität Dresden
• 依托单位国家: 德国
• 项目类别: Major Research Instrumentation
• 财政年份: 2023
• 资助国家: 德国
• 起止时间: 2022-12-31 至 无数据
• 项目状态: 未结题
• 来源: https://gepris.dfg.de/gepris/projekt/521411486?language=en
• 关键词: 600; MHz; NMR; spectrometer

A modern 600 MHz liquid NMR spectrometer with a nitrogen-cooled cryo probe head with a "normal" coil arrangement (X inside, 1H/19F outside) is proposed. The use of cryo technology improves the signal-to-noise ratio by a factor of three compared to room temperature probes. With a given amount of substance, not only can significant measurement time reductions be achieved, but more complex NMR measurement methods in the field of 2D NMR spectroscopy with significantly reduced measurement times can also be used. Due to the geometry of the probe head (internal 13C coil), this device will represent a significant gain, especially in the structural elucidation of highly substituted natural and active substances that are characterized by a high level of quaternary carbon atoms. Furthermore, polyaromatic systems, such as those used primarily in the field of materials science and which are also characterized by a large number of quaternary carbon atoms, can be characterized much better. Another method that is particularly useful in the field of biosynthesis elucidation of new natural products (here also using INADEQUATE), the metabolic degradation of active substances, as well as in the field of mechanism elucidation is based on the shifting of 13C signals by isotope labeling (e.g. 2H, 15N, 18O). Due to the high 13C sensitivity, which is achieved by the cryo probe head, not only isotope labels can be determined with exact position via 13C NMR spectra. Rather, the isotope content can also be quantified by integrating the 13C signals from labeled carbon atoms. Finally, the device opens up the possibility of direct measurement of a kinetic isotope effect, e.g. by 1H-13C polarization transfer measurements, which is complementary to the method described above.

提出了一种现代 600 MHz 液体核磁共振波谱仪，配有氮冷却低温探头，具有“正常”线圈排列（X 内部，1H/19F 外部）。与室温探头相比，低温技术的使用将信噪比提高了三倍。对于给定量的物质，不仅可以显着缩短测量时间，而且还可以使用 2D NMR 波谱领域中更复杂的 NMR 测量方法，从而显着缩短测量时间。由于探头（内部 13C 线圈）的几何形状，该设备将带来显着的增益，特别是在以高水平季碳原子为特征的高度取代的天然活性物质的结构阐明方面。此外，可以更好地表征聚芳族系统，例如主要用于材料科学领域且也以大量季碳原子为特征的聚芳族系统。另一种在新天然产物的生物合成阐明领域（此处也使用 INADEQUATE）、活性物质的代谢降解以及机制阐明领域特别有用的方法是基于通过同位素标记转移 13C 信号（例如 2H、15N、18O）。由于冷冻探针头实现了高 13C 灵敏度，因此不仅可以通过 13C NMR 光谱确定同位素标记的精确位置。相反，同位素含量也可以通过整合标记碳原子的 13C 信号来量化。最后，该设备开启了直接测量动力学同位素效应的可能性，例如通过 1H-13C 偏振传输测量，这是对上述方法的补充。