Solid-State NMR/Dynamic Nuclear Polarization of Polypeptides in Planar Supported Lipid Bilayers.

摘要: Dynamic nuclear polarization has been developed to overcome the limitations of inherently low signal intensity NMR spectroscopy. This technique promises be particularly useful for solid-state spectroscopy where signals are broadened over a larger frequency range and most investigations rely on recording gamma nuclei. To extend possible investigations, triple-resonance flat-coil probe is presented with microwave irradiation capacities allowing investigation static samples at temperatures 100 K, including supported lipid bilayers. The performance allows two-dimensional separated local field experiments high-power Lee-Goldberg decoupling cross-polarization under simultaneous from gyrotron generator. Efficient cooling sample turned out essential best enhancements line shape necessitated development dedicated chamber. Furthermore, new membrane-anchored biradical presented, geometry membranes was optimized not only good membrane alignment, handling, stability, filling factor coil but also heat dissipation. Enhancement factors 17-fold were obtained, PISEMA spectrum transmembrane helical peptide obtained in less than 2 h.