Hydration and Temperature Dependence of 13C and 1H NMR Spectra of the DMPC Phospholipid Membrane and Complete Resonance Assignment of Its Crystalline State
Hydration and Temperature Dependence of 13C and 1H NMR Spectra of the DMPC Phospholipid Membrane and Complete Resonance Assignment of Its Crystalline State
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DOI：
10.1021/jp208958a
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发表时间：
2011-12-22
影响因子：
3.3
通讯作者：
Morigaki, Kenichi
中科院分区：
文献类型：
--
作者：
Nomura, Kaoru;Lintuluoto, Masami;Morigaki, Kenichi
分子构象分布引起的非均匀谱线加宽是固体核磁共振波谱研究中的难题之一。避免它的最好方法是使样品结晶。在这里，我们提出了高有序晶体1,2-二myrystoyl- sr -glycero-3-phosphocholine （DMPC）的高分辨率C-13交叉极化（CP）魔角旋转（MAS）核磁共振波谱，并使用二维（2D）固态核磁共振波谱、偶极异核相关（hetor）波谱、基于标量异核J耦合的化学位移相关（MAS-J- hmqc）波谱和偶极辅助旋转共振（DARR）波谱对其进行了完全分配。本研究固体核磁共振计算的化学位移值与x射线晶体DMPC结构的计算化学位移值比较，结果吻合较好，表明晶体DMPC中的两种异构体与x射线晶体结构具有相同的构象。低水化水平DMPC(3)的相图
Inhomogeneous line broadening due to conformational distributions of molecules is one of the troublesome problems in solid-state NMR spectroscopy. The best possible way to avoid it is to crystallize the sample. Here, we present a highly resolved C-13 cross-polarization (CP) magic angle spinning (MAS) NMR spectrum of the highly ordered crystalline 1,2-dimyrystoyl-sn-glycero-3-phosphocholine (DMPC) and completely assigned it using two-dimensional (2D) solid-state NMR spectra, dipolar heteronuclear correlation (HETCOR) spectra, scalar heteronuclear J coupling based chemical shift correlation (MAS-J-HMQC) spectra, and Dipolar Assisted Rotational Resonance (DARR) spectra. A comparison between assigned chemical shift values by solid-state NMR in this study and the calculated chemical shift values for X-ray crystal DMPC structures shows good agreement, indicating that the two isomers in the crystalline DMPC take the same conformation as the X-ray crystal structure. The phase diagram of the low hydration level of DMPC (3