Pushing Boundaries in Solid-State NMR Research

The CryoProbe technology has significantly impacted solution-state nuclear magnetic resonance (NMR). Following over 25 years of continual upgrades and developments, the CryoProbe has become broadly implemented in NMR laboratories internationally (Kovacs & Moskau, 2013).

a picture of an NMR tool in use

Image Credit: smereka/Shutterstock.com

Sensitivity improvements of up to four alongside equivalent room temperature (RT) probes have been reported on numerous sample types, facilitating investigational time savings of up to an order of magnitude.

This significant increase in productivity has enabled many academic and industrial research groups to equip a CryoProbe in their laboratories.

The technology’s success drove its extension into Magnetic Resonance Imaging and later, solid-state NMR. In 2019, Bruker introduced a commercial triple-resonance 600 MHz MAS CryoProbe exclusively developed for structural biology uses—a first in the industry.

Bruker’s MAS CryoProbe range has been recently expanded with a double resonance probe fitted with a broadband channel, specially created to offer novel solutions in material science.

The double resonance MAS CryoProbe is the most recent addition to the CryoProbe family. Few of these devices exist globally in industrial and academic NMR laboratories.

Like the liquid CryoProbes, the MAS CryoProbe provides a typical mass sensitivity enhancement factor of 3-4 compared with comparable room-temperature probes, offering a significant increase in sensitivity.

Heightened sensitivity enables faster spectral recording and delivers additional investigational benefits like recording more dimension for enhanced resolution.

Another benefit of increased sensitivity is the capacity to study dilute samples, with concentrations typically under the detection limit of typical RT probes. This sensitivity boost can also be applied to studying native samples or samples with lower labeling amounts, successfully lowering the price of producing samples.

Making a cryogenically cooled probe for solid-state NMR poses distinctive challenges, including:

  • Highly demanding RF field performance
  • Requiring efficient thermal isolation between the sample and probe circuitry’s cryogenic components
  • Sample accessibility
  • Magic angle adjustment
  • Spinning stability causes significant technical demands

Bruker has accomplished equal outstanding performance requirements and practical constraints. The MAS CryoProbe is revolutionary in solid-state NMR.

This article demonstrates Bruker’s cooperative efforts with clients, utilizing the MAS CryoProbe to examine challenging samples. The work is vast, from biological systems to material science and pharmaceuticals.

Some samples are initially studied at natural abundance level. Other samples contain numerous isotopically enriched spin systems, on which multiple-dimension high-quality experiments were initially acquired.

Insensitive nuclei including 47Ti, 49Ti, 25Mg, and 67Zn were evaluated using the 800 MHz double resonance low gamma MAS CryoProbe.

The results are presented concisely to highlight the versatility of the MAS CryoProbe in producing unprecedented data.

Image

This information has been sourced, reviewed and adapted from materials provided by Bruker BioSpin - NMR, EPR and Imaging.

For more information on this source, please visit Bruker BioSpin - NMR, EPR and Imaging.

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