Band-selective heteronuclear dipolar recoupling with dual back-to-back pulses in rotating solids.
We propose a robust band-selective heteronuclear15N-13C recoupling method using dual back-to-back (BABA) pulses (DBP). It contains four 90° pulses in each rotor period and corresponding phase cycling on each channel (13C and15N). DBP aims at rapid band-selective heteronuclear magnetization transfer between15N and13Cα/13C', whose efficiency is close to that of the well-known SPECIFIC CP in membrane proteins with relatively short relaxation time in rotating frame (T1ρ). Compared to SPECIFIC CP, DBP is very simple to set up and highly robust to RF variations. Thus, it can reduce the efforts in experimental optimization, especially for low-sensitive samples, and is very suitable for long-time or quantitative experiments. The efficacy of DBP is demonstrated by the E. coli diacylglycerol kinase (DAGK) proteoliposome. We anticipate that DBP would be useful for (segments of) membrane proteins that undergo the μs-ms timescale motions in magic-angle spinning (MAS) solid-state NMR.
National Center for Magnetic Resonance in Wuhan, Key Laboratory of Magnetic Resonance in Biological Systems, State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, Wuhan 430071, PR China.
Zhengfeng
Z
Zhang
National Center for Magnetic Resonance in Wuhan, Key Laboratory of Magnetic Resonance in Biological Systems, State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, Wuhan 430071, PR China.
Yanke
Y
Chen
National Center for Magnetic Resonance in Wuhan, Key Laboratory of Magnetic Resonance in Biological Systems, State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, Wuhan 430071, PR China. Electronic address: yangjun@wipm.ac.cn.
Jun
J
Yang
Band-selective; Double cross polarization (DCP); Dual back-to-back pulses (DBP); Heteronuclear recoupling; Magic-angle spinning (MAS) solid-state NMR; Membrane proteins; Relaxation time in rotating frame (T(1ρ)); SPECIFIC CP