experiment for 1H CP-HSQC at fast MAS.

This 2D experiment measures 1H - 13C crosscorrelation CP-HSQC at fast MAS (1.3mm probe at 60kHz spinning frequency).

Citation

https://www.ncbi.nlm.nih.gov/pubmed/25102442 E. Barbet-Massin, A.J. Pell, J.S. Retel, et al., Rapid Proton-Detected NMR Assignment for Proteins with Fast Magic Angle Spinning., JACS 136 (35), pp 12489-12497 (2014).

Sample heating

Frictional heating during ultra fast spinning may heat up a sample by up to 40K.

Citation

[https://www.biorxiv.org/content/10.1101/566729v1.full] TmDOTP : An NMR- based Thermometer for Magic Angle Spinning NMR Experiments Dongyu Zhang, Boris Itin, Ann E. McDermott; preprinted

Protocol

Optimize both CP segments using the sample of interest. Literature recommends using 10% linear ramps, the author finds 20% tangential ramps to perform better.

Samples

The experiments were performed with a precipitated microcrystalline u-13C,15N labeled protein

Processing and analysis

Fourier transform a 2D experiment. Gaussian apodization is recommended.

Pulse Sequence and Parameter Set