Rapid 3D NMR using the filter diagonalization method: application to oligosaccharides derivatized with (13)C-labeled acetyl groups.

Armstrong GS, Cano KE, Mandelshtam VA, Shaka AJ, Bendiak B.

Chemistry Department, University of California, Irvine, CA 92697-2025, USA.

Rapid 3D NMR spectroscopy of oligosaccharides having isotopically labeled acetyl "isotags" was made possible with high resolution in the indirect dimensions using the filter diagonalization method (FDM). A pulse sequence was designed for the optimal correlation of acetyl methyl protons, methyl carbons, and carbonyl carbons. The multi-dimensional nature of the FDM, coupled with the advantages of constant-time evolution periods, resulted in marked improvements over Fourier transform (FT) and mirror-image linear prediction (MI-LP) processing methods. The three methods were directly compared using identical data sets. A highly resolved 3D spectrum was achieved with the FDM using a very short experimental time (28min).