Towards complete suppression of diagonal peaks in solid-state MAS NMR homonuclear chemical shift correlation spectra.

The feasibility of applying the spin-echo based diagonal peak suppression method in solid-state MAS NMR homonuclear chemical shift correlation experiments is demonstrated. A complete phase cycling is designed to generate sine- and cosine-modulations of the chemical shift difference between the spin-diffused signals, enabling the quadrature detection in the indirect dimension. Meanwhile, all signals not involved in polarization transfer are refocused at the center of the indirect dimension. A data processing algorithm is developed to extract and suppress these spin-echo refocused signals without affecting nearby spin-diffused cross peaks. The processed spectrum is then converted into a conventional two-dimensional homonuclear chemical shift correlation spectrum, free of diagonal peaks. The effectiveness of this method is illustrated using a uniformly C-labeled Fmoc-leucine sample and a sample of human Atg8 homolog LC3B, directly conjugated to the amino headgroup of phosphatidylethanolamine (PE) lipids in liposomes.