CNRS/ENS Lyon/UCB Lyon 1, Centre de RMN à Très Hauts Champs, University of Lyon, Villeurbanne, France.
J Biomol NMR. 2013 Aug;56(4):379-86. doi: 10.1007/s10858-013-9757-3. Epub 2013 Jun 29.
We present here (1)H-detected triple-resonance H/N/C experiments that incorporate CO-CA and CA-CB out-and-back scalar-transfer blocks optimized for robust resonance assignment in biosolids under ultra-fast magic-angle spinning (MAS). The first experiment, (H)(CO)CA(CO)NH, yields (1)H-detected inter-residue correlations, in which we record the chemical shifts of the CA spins in the first indirect dimension while during the scalar-transfer delays the coherences are present only on the longer-lived CO spins. The second experiment, (H)(CA)CB(CA)NH, correlates the side-chain CB chemical shifts with the NH of the same residue. These high sensitivity experiments are demonstrated on both fully-protonated and 100%-H(N) back-protonated perdeuterated microcrystalline samples of Acinetobacter phage 205 (AP205) capsids at 60 kHz MAS.
我们在此展示了（1）H 检测的三共振 H/N/C 实验，该实验结合了 CO-CA 和 CA-CB 往返标量转移模块，经过优化，可在超快魔角旋转（MAS）下对生物固体中的共振分配进行稳健赋值。第一个实验（H）（CO）CA（CO）NH 产生了（1）H 检测的残基间相关，其中我们记录了第一个间接维度中 CA 自旋的化学位移，而在标量转移延迟期间，相干性仅存在于寿命更长的 CO 自旋上。第二个实验（H）（CA）CB（CA）NH 将侧链 CB 化学位移与同一残基的 NH 相关联。这些高灵敏度实验是在 60 kHz MAS 下对完全质子化和 100%H（N）反质子化的去氘微结晶 Acinetobacter phage 205（AP205）衣壳的样品上进行的。
