Cryo-coil MAS H/ C/ H/ N/ Probe for Highest S/N in NMR

描述（由申请人提供）： 三十多年来，高分辨率（HR）核磁共振（NMR）一直是一种领先的分析技术，用于在均相体系中阐明所有类型的分子（无论大小）的结构和功能。最近，魔角旋转（MAS）已与高场HRNMR相结合，将该技术扩展到非均匀系统，如人类和动物组织。恶性乳腺癌组织的1H HRMAS光谱显示与非恶性乳腺组织相比磷酸胆碱水平显著增加，并且如果HR-MAS探针的信噪比（SNR）可以充分增加，则似乎可以鉴定许多其他病理的其他明确标记物。MAS也被成千上万的NMR研究人员用于大分子结构测定、有机金属络合物和膜蛋白等领域。 用于液体的HR NMR探头最近已可与低温冷却样品线圈一起使用，由于其SNR的四分之一改善，这些线圈正在彻底改变NMR领域。在HR-MAS中，SNR的类似改进是可能的。开发低温线圈HR-MAS探头的工程挑战是巨大的，但并非不可克服。详细的电路分析、全波电磁线圈分析、计算流体动力学（CFD）、热模拟和MAS实验表明：（1）四谐振MAS的新方法（1H/13 C/2 H/15 N），所有关键电路元件保持在25 K附近，（2）将陶瓷杜瓦瓶集成到新型样品旋转器系统中，和（3）低温超导体提供了在至少高达14 T（600 MHz）的磁场下低温线圈HR-MAS探针中SNR增加四倍的潜力。第一阶段已经证明了具有高效四谐振低温电路的bewared MAS旋转器设计的技术可行性，其信号采集时间减少了一个数量级以上。第二阶段将完成四共振冷冻线圈HR-MAS的必要开发，脉冲场梯度高达14 T。在格鲁吉亚大学的初步实地测试预计在第二阶段进行到一半。第二阶段之后的后续工作预计将把该技术扩展到800 MHz。

DESCRIPTION (provided by applicant): For over three decades, High-Resolution (HR) Nuclear Magnetic Resonance (NMR) has been a leading analytical technique for structure and function elucidation of molecules of all types, large and small, in homogeneous systems. More recently, Magic Angle Spinning (MAS) has been combined with high-field HRNMR to extend the technique to inhomogeneous systems, such as human and animal tissues. The 1H HRMAS spectrum of malignant breast cancer tissue shows dramatically increased levels of phosphocholine compared to nonmalignant breast tissue, and it appears likely that other unambiguous markers can be identified for many other pathologies if the signal to noise ratio (SNR) of the HR-MAS probe can be increased sufficiently. MAS is also utilized by thousands of NMR researchers in fields such as macromolecule structure determination, organo-metallo-complexes, and membrane proteins. HR NMR probes for liquids have recently become available with cryogenically cooled sample coils that are revolutionizing the field of NMR owing to their factor-of-four improvement in SNR. Similar improvements in SNR may be possible in HR-MAS. The engineering challenges of developing a cryo-coil HR-MAS probe are enormous, but not insurmountable. Detailed circuit analysis, full-wave electromagnetic coil analysis, computational fluid dynamics (CFD), thermal simulations, and MAS experiments show that a combination of (1) a novel approach to quad-resonance MAS (IH/13C/2H/15N) with all of the critical circuit elements maintained near 25K, (2) integrating a ceramic dewar into a novel sample spinner system, and (3) cryogenic preamps offers the potential for a factor-of-four increase in SNR in a cryo-coil HR-MAS probe at fields at least up to 14T (600 MHz). The Phase I has demonstrated technical feasibility of a bewared MAS spinner design with a high-efficiency quad-resonance cryogenic circuit for more than an order-of-magnitude reduction in signal acquisition time. Phase II will complete the developments necessary for quad-resonance cryo-coil HR-MAS with pulsed-field gradients at fields up to 14T. Initial field-testing at the University of Georgia is expected midway through the Phase II. Subsequent work following this Phase II is expected to extend the technology to 800 MHz.