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E H Hardy

Publications and source records attributed to E H Hardy.

2 recordsLinked to original sources
PubMed2001

Fast MAS total through-bond correlation spectroscopy.

Mixing sequences for total through-bond correlation spectroscopy in solids (TOBSY) were developed. The motivation is the design of broadband, effective, and robust sequences adapted for "fast" MAS. Possible sequences with the desired Hamiltonian (the homonuclear isotropic J interaction) were identified using lowest order average Hamiltonian theory. Numerical simulations as a function of the MAS frequency were then employed to further characterize the performance. An experimental TOBSY spectrum of a uniformly (13)C-labeled decapeptide at 20 kHz MAS was obtained using one of the new sequences. The spectrum allows us to assign the (13)C resonances to the respective spin systems.

Journal Article↗
PubMed2001

Methods for sequential resonance assignment in solid, uniformly 13C, 15N labelled peptides: quantification and application to antamanide.

The application of adiabatic polarization-transfer experiments to resonance assignment in solid, uniformly 13C-15N-labelled polypeptides is demonstrated for the cyclic decapeptide antamanide. A homonuclear correlation experiment employing the DREAM sequence for adiabatic dipolar transfer yields a complete assignment of the C(alpha) and aliphatic side-chain 13C resonances to amino acid types. The same information can be obtained from a TOBSY experiment using the recently introduced P9(12)1 TOBSY sequence, which employs the J couplings as a transfer mechanism. A comparison of the two methods is presented. Except for some aromatic phenylalanine resonances, a complete sequence-specific assignment of the 13C and 15N resonances in antamanide is achieved by a series of selective or broadband adiabatic triple-resonance experiments. Heteronuclear transfer by adiabatic-passage Hartmann-Hahn cross polarization is combined with adiabatic homonuclear transfer by the DREAM and rotational-resonance tickling sequences into two- and three-dimensional experiments. The performance of these experiments is evaluated quantitatively.

Amino Acids↗