Nuzillard Jean-Marc
Centre National de la Recherche Scientifique, Institut de Chimie Moléculaire de Reims, REIMS Cedex 2, France.
J Magn Reson. 2008 Feb;190(2):292-7. doi: 10.1016/j.jmr.2007.11.011. Epub 2007 Nov 22.
The biselective spin echo technique allows the signals of coupled proton pairs to be extracted from crowded liquid state proton NMR spectra. Its use as a preparation sequence in heteronuclear chemical shift correlation experiments requires the removal of the heteronuclear coupling interaction during the biselective echo time. The discrimination between coupled and uncoupled protons signals is achieved by double quantum filtration, which delivers antiphase magnetization states. The latter are not directly compatible with the design of an HSQC-like pulse sequence. The conversion of antiphase to in-phase magnetization states by a second biselective echo sequence solves this problem. The optimization of spin echo delays is also discussed. Lastly, the article presents modified HSQC and HMBC pulses sequences in which information is obtained solely for the biselectively selected proton pairs. A peracetylated trisaccharide was used as a test molecule.
双选择性自旋回波技术能够从拥挤的液态质子核磁共振谱中提取耦合质子对的信号。将其用作异核化学位移相关实验中的制备序列时,需要在双选择性回波时间内消除异核耦合相互作用。通过双量子滤波实现对耦合质子信号与非耦合质子信号的区分,双量子滤波可产生反相磁化态。而后者与类似HSQC脉冲序列的设计并不直接兼容。通过第二个双选择性回波序列将反相磁化态转换为同相磁化态可解决此问题。文中还讨论了自旋回波延迟的优化。最后,本文介绍了改进的HSQC和HMBC脉冲序列,其中仅针对双选择性选择的质子对获取信息。使用全乙酰化三糖作为测试分子。