Alam T M, Holland G P
Department of Electronic and Nanostructured Materials, Sandia National Laboratories, Albuquerque, NM 87185, USA.
J Magn Reson. 2006 Jun;180(2):210-21. doi: 10.1016/j.jmr.2006.02.013. Epub 2006 Mar 24.
Two-dimensional (1)H-(13)C INEPT MAS NMR experiments utilizing a (1)H-(1)H magnetization exchange mixing period are presented for characterization of lipid systems. The introduction of the exchange period allows for structural information to be obtained via (1)H-(1)H dipolar couplings but with (13)C chemical shift resolution. It is shown that utilizing a RFDR recoupling sequence with short mixing times in place of the more standard NOE cross-relaxation for magnetization exchange during the mixing period allowed for the identification and separation of close (1)H-(1)H dipolar contacts versus longer-range inter-molecular (1)H-(1)H dipolar cross-relaxation. These 2D INEPT experiments were used to address both intra- and inter-molecular contacts in lipid and lipid/cholesterol mixtures.
提出了利用¹H-¹H磁化交换混合期的二维¹H-¹³C异核多量子相干(INEPT)固体核磁共振(NMR)实验来表征脂质体系。交换期的引入使得能够通过¹H-¹H偶极耦合获得结构信息,但具有¹³C化学位移分辨率。结果表明,在混合期利用具有短混合时间的旋转框架双共振(RFDR)重耦合序列代替更标准的用于磁化交换的核Overhauser效应(NOE)交叉弛豫,能够识别和区分近距离的¹H-¹H偶极接触与长程分子间¹H-¹H偶极交叉弛豫。这些二维INEPT实验用于研究脂质和脂质/胆固醇混合物中的分子内和分子间接触。