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.

提出了一种现代的600 MHz液体NMR光谱仪，其带有“正常”线圈布置的氮气冷冻探针头（X内部，1H/19F外部）。与室温探针相比，冷冻技术的使用可提高信噪比的三倍。使用给定数量的物质，不仅可以实现大幅度的测量时间缩短，而且还可以使用2D NMR光谱的领域中更复杂的NMR测量方法，并可以使用大幅减少的测量时间。由于探针头的几何形状（内部13C线圈），该设备将代表显着的增益，尤其是在结构化高度取代的天然和活性物质的结构上，这些物质的特征是高水平的Quaternary碳原子。此外，可以更好地表征多芳烃系统，例如主要用于材料科学领域的多野药系统，也以大量第四纪碳原子为特征。另一种在新天然产物的生物合成领域特别有用的方法（此处也使用不充分），活性物质的代谢降解以及阐明的机理领域基于同位素标记对13C信号的转移（例如2H，15N，15N，18O）。由于高13C敏感性，这是由冷冻探针头实现的，不仅可以通过13C NMR光谱确切地确定同位素标签。相反，同位素含量也可以通过整合来自标记的碳原子的13C信号来量化。最后，该设备打开了直接测量动力学同位素效应的可能性，例如通过1H-13C极化转移测量值，这与上述方法互补。