Physical Chemistry, ETH Zürich, Wolfgang-Pauli-Strasse 10, 8093 Zürich, Switzerland.
Center for Insoluble Protein Structures (inSPIN), Interdisciplinary Nanoscience Center (iNANO) and Department of Chemistry, Aarhus University, Gustav Wieds Vej 14, DK-8000 Aarhus C, Denmark.
J Magn Reson. 2013 Dec;237:147-151. doi: 10.1016/j.jmr.2013.09.002. Epub 2013 Oct 11.
We present a new dipolar recoupling method for efficient and robust heteronuclear polarization transfer in solid-state NMR under magic-angle-spinning (MAS) conditions. The method combines the recent (RESPIRATION)CP method with a modulation of the amplitude of the rotor-synchronized pulses at one of the involved rf channels through the recoupling condition. In this manner, it is possible to achieve high transfer efficiencies while maintaining robustness towards rf-field inhomogeneities and resonance offsets. The performance of the so-called adiabatic-(RESPIRATION)CP experiment is demonstrated numerically and experimentally using uniformly (13)C,(15)N-labeled samples of alanine and ubiquitin. In particular for cases with relatively high rf inhomogeneity, the scheme offers advantages over the commonly used dipolar recoupling pulse sequences.
我们提出了一种新的偶极子重聚方法,用于在魔角旋转(MAS)条件下实现固态 NMR 中有效的和稳健的异核极化转移。该方法将最近的(RESPIRATION)CP 方法与通过重聚条件调制涉及的其中一个射频通道的转子同步脉冲的幅度相结合。通过这种方式,可以在保持对射频场不均匀性和共振偏移的稳健性的同时,实现高效率的转移。使用均匀(13)C,(15)N 标记的丙氨酸和泛素样品,通过数值和实验证明了所谓的绝热-(RESPIRATION)CP 实验的性能。特别是对于射频不均匀性相对较高的情况,该方案优于常用的偶极子重聚脉冲序列。