Inductively coupled magic angle spinning microresonators benchmarked for high-resolution single embryo metabolomic...

Area of Science:

• Nuclear Magnetic Resonance (NMR) Spectroscopy
• Solid-State Chemistry
• Biochemistry

Background:

• Magic Angle Coil Spinning (MACS) offers significant sensitivity enhancements for solid-state NMR.
• Widespread adoption of MACS has been limited by issues like spectral linewidth, eddy current heating, and manufacturing imprecision.
• Previous MACS technology was not ideal for studying live biological samples or for large-scale use.

Purpose of the Study:

• To develop and present a novel device that overcomes the limitations of previous MACS technology.
• To achieve high spectral resolution and sensitivity for mass-limited samples.
• To enable the study of live biological samples and facilitate metabolomic research.

Main Methods:

• Development of a new MACS device using wafer-scale fabrication for reproducible inserts.
• Characterization of spectral resolution and limit of detection using sucrose standards.
• Measurement of temperature increase within the MACS insert under specific magnetic field and spinning conditions.
• Application of the device for high-resolution J-coupling measurements and single zebrafish embryo NMR studies.

Main Results:

• Achieved spectral resolution of approximately 0.01 ppm and a normalized limit of detection of approximately 13 nmol s^0.5.
• Demonstrated a limited temperature increase of only 5 °C at 5 kHz MAS frequency in a 11.74 T magnetic field.
• Successfully resolved ultra-fine 1H-1H and 13C-13C J-couplings in 10 minutes for a 13C-labeled glucose sample.
• Acquired 1H-1H COSY spectra from a single zebrafish embryo within 4.5 hours.

Conclusions:

• The new MACS device significantly improves spectral resolution, sensitivity, and thermal stability, addressing key limitations of prior technology.
• Wafer-scale fabrication ensures reproducible MACS inserts, promoting broader adoption in biochemistry and metabolomics.
• The demonstrated capabilities open new avenues for studying precious biological samples, including single-cell and single-embryo NMR analyses.