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.

本文提出了一种新型的600 MHz液体核磁共振谱仪，它采用了一种“常规”线圈排列（X内，1H/19 F外）的氮冷低温探头。与室温探头相比，低温技术的使用将信噪比提高了三倍。在给定量的物质的情况下，不仅可以实现显著的测量时间减少，而且还可以使用具有显著减少的测量时间的2D NMR光谱学领域中的更复杂的NMR测量方法。由于探头的几何形状（内部13 C线圈），该设备将代表一个显着的增益，特别是在结构解析的高度取代的天然和活性物质，其特征是高水平的季碳原子。此外，聚芳族体系，例如主要用于材料科学领域并且也以大量季碳原子为特征的那些，可以更好地表征。在新天然产物的生物合成阐明领域（这里也使用INADEQUATE）、活性物质的代谢降解以及机理阐明领域中特别有用的另一种方法是基于通过同位素标记（例如2 H、15 N、18 O）的13 C信号的移位。由于低温探头具有高13 C灵敏度，因此不仅可以通过13 C NMR光谱确定同位素标记的准确位置。相反，同位素含量也可以通过整合来自标记碳原子的13 C信号来定量。最后，该装置开启了直接测量动力学同位素效应的可能性，例如通过1H-13 C极化转移测量，这是对上述方法的补充。