title: Simultaneous cross polarization to (13)C and (15)N with (1)H detection at 60kHz MAS solid-state NMR.
abstract: We describe high resolution MAS solid-state NMR experiments that utilize (1)H detection with 60kHz magic angle spinning; simultaneous cross-polarization from (1)H to (15)N and (13)C nuclei; bidirectional cross-polarization between (13)C and (15)N nuclei; detection of both amide nitrogen and aliphatic carbon (1)H; and measurement of both (13)C and (15)N chemical shifts through multi-dimensional correlation experiments. Three-dimensional experiments correlate amide (1)H and alpha (1)H selectively with (13)C or (15)N nuclei in a polypeptide chain. Two separate three-dimensional spectra correlating (1)Hα/(13)Cα/(1)H(N) and (1)H(N)/(15)N/(1)Hα are recorded simultaneously in a single experiment, demonstrating that a twofold savings in experimental time is potentially achievable. Spectral editing using bidirectional coherence transfer pathways enables simultaneous magnetization transfers between (15)N, (13)Cα(()(i)()) and (13)C'(()(i)(-1)), facilitating intra- and inter-residue correlations for sequential resonance assignment. Non-uniform sampling is integrated into the experiments, further reducing the length of experimental time.
authors.affiliation: Department of Chemistry and Biochemistry, University of California, San Diego, La Jolla, CA 92093, USA.
authors.forename: Bibhuti B
authors.initials: BB
authors.lastname: Das
authors.affiliation: Department of Chemistry and Biochemistry, University of California, San Diego, La Jolla, CA 92093, USA. Electronic address: sopella@ucsd.edu.
authors.forename: Stanley J
authors.initials: SJ
authors.lastname: Opella
mesh_terms: D000577:Amides / Q000737:chemistry; D017104:Bacteriophage M13 / Q000737:chemistry; D036022:Capsid Proteins / Q000737:chemistry; D002247:Carbon Isotopes; D009587:Nitrogen Isotopes; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods*; D009842:Oligopeptides / Q000737:chemistry; D010455:Peptides / Q000737:chemistry; D011506:Proteins / Q000737:chemistry; D011522:Protons
chemical_list: D000577:Amides; D036022:Capsid Proteins; D002247:Carbon Isotopes; D009587:Nitrogen Isotopes; D009842:Oligopeptides; D010455:Peptides; D011506:Proteins; D011522:Protons
keywords: Dual observation; Magic angle spinning; Peptides; Proteins; Triple-resonance