Dataset Information

Enhancing NMR Sensitivity of Natural-Abundance Low-? Nuclei by Ultrafast Magic-Angle-Spinning Solid-State NMR Spectroscopy.

ABSTRACT: Although magic-angle-spinning (MAS) solid-state NMR spectroscopy has been able to provide piercing atomic-level insights into the structure and dynamics of various solids, the poor sensitivity has limited its widespread application, especially when the sample amount is limited. Herein, we demonstrate the feasibility of acquiring high S/N ratio natural-abundance 13 C?NMR spectrum of a small amount of sample (?2.0?mg) by using multiple-contact cross polarization (MCP) under ultrafast MAS. As shown by our data from pharmaceutical compounds, the signal enhancement achieved depends on the number of CP contacts employed within a single scan, which depends on the T1? of protons. The use of MCP for fast 2D 1 H/13 C heteronuclear correlation experiments is also demonstrated. The significant signal enhancement can be greatly beneficial for the atomic-resolution characterization of many types of crystalline solids including polymorphic drugs and nanomaterials.

SUBMITTER: Zhang R

PROVIDER: S-EPMC5831690 | biostudies-literature | 2016 Oct

REPOSITORIES: biostudies-literature

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Publications

Enhancing NMR Sensitivity of Natural-Abundance Low-γ Nuclei by Ultrafast Magic-Angle-Spinning Solid-State NMR Spectroscopy.

Zhang Rongchun R Chen Yitian Y Rodriguez-Hornedo Nair N Ramamoorthy Ayyalusamy A

Chemphyschem : a European journal of chemical physics and physical chemistry 20160722 19

Although magic-angle-spinning (MAS) solid-state NMR spectroscopy has been able to provide piercing atomic-level insights into the structure and dynamics of various solids, the poor sensitivity has limited its widespread application, especially when the sample amount is limited. Herein, we demonstrate the feasibility of acquiring high S/N ratio natural-abundance <sup>13</sup> C NMR spectrum of a small amount of sample (≈2.0 mg) by using multiple-contact cross polarization (MCP) under ultrafast MA ...[more]

PMID: 27310287

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Project description:Solid-state NMR spectroscopy is one of the most commonly used techniques to study the atomic-resolution structure and dynamics of various chemical, biological, material, and pharmaceutical systems spanning multiple forms, including crystalline, liquid crystalline, fibrous, and amorphous states. Despite the unique advantages of solid-state NMR spectroscopy, its poor spectral resolution and sensitivity have severely limited the scope of this technique. Fortunately, the recent developments in probe technology that mechanically rotate the sample fast (100 kHz and above) to obtain "solution-like" NMR spectra of solids with higher resolution and sensitivity have opened numerous avenues for the development of novel NMR techniques and their applications to study a plethora of solids including globular and membrane-associated proteins, self-assembled protein aggregates such as amyloid fibers, RNA, viral assemblies, polymorphic pharmaceuticals, metal-organic framework, bone materials, and inorganic materials. While the ultrafast-MAS continues to be developed, the minute sample quantity and radio frequency requirements, shorter recycle delays enabling fast data acquisition, the feasibility of employing proton detection, enhancement in proton spectral resolution and polarization transfer efficiency, and high sensitivity per unit sample are some of the remarkable benefits of the ultrafast-MAS technology as demonstrated by the reported studies in the literature. Although the very low sample volume and very high RF power could be limitations for some of the systems, the advantages have spurred solid-state NMR investigation into increasingly complex biological and material systems. As ultrafast-MAS NMR techniques are increasingly used in multidisciplinary research areas, further development of instrumentation, probes, and advanced methods are pursued in parallel to overcome the limitations and challenges for widespread applications. This review article is focused on providing timely comprehensive coverage of the major developments on instrumentation, theory, techniques, applications, limitations, and future scope of ultrafast-MAS technology.

Dataset Information

Enhancing NMR Sensitivity of Natural-Abundance Low-? Nuclei by Ultrafast Magic-Angle-Spinning Solid-State NMR Spectroscopy.

Publications

Enhancing NMR Sensitivity of Natural-Abundance Low-γ Nuclei by Ultrafast Magic-Angle-Spinning Solid-State NMR Spectroscopy.

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