Rapid high-resolution four-dimensional NMR spectroscopy using the filter diagonalization method and its advantages for detailed structural elucidation of oligosaccharides
Rapid high-resolution four-dimensional NMR spectroscopy using the filter diagonalization method and its advantages for detailed structural elucidation of oligosaccharides
复制标题
DOI：
10.1016/j.jmr.2004.11.027
复制
发表时间：
2005-03-01
影响因子：
2.2
通讯作者：
Bendiak, B
中科院分区：
文献类型：
--
作者：
Armstrong, GS;Mandelshtam, VA;Bendiak, B
作为滤波对角化方法（FDM）的一种实现，报道了具有间接维度高分辨率信号的四维核磁共振波谱。使用由c -13标记的乙酰基同位标签衍生的低聚糖，定制了一个与FDM联合使用的四维恒定时间脉冲序列。结果表明，尽管光谱在直接和所有三个间接维度上高度拥挤，但在相对较短的实验时间内（19 h）可以实现所有维度的高分辨率。结合使用等标签、恒定时间脉冲序列和FDM，可以在多个维度上快速分离糖环质子自旋系统，并且可以简单地测量所有的内环j -偶联，这是分配糖体化学和异构构型的关键目标。一种快速、明确地阐明低聚糖自旋体系的通用方法一直是碳水化合物NMR长期追求的目标，而与FDM相结合的等位标签现在使这一目标很容易实现。强调了FDM程序用于从四维光谱生成任何维度的高分辨率二维切片的其他一般优点。(C) 2004爱思唯尔公司版权所有。
Four-dimensional nuclear magnetic resonance spectroscopy with high resolution of signals in the indirect dimensions is reported as an implementation of the filter diagonalization method (FDM). Using an oligosaccharide derivatized with C-13-labeled acetyl isotags, a four-dimensional constant-time pulse sequence was tailored for conjoint use with the FDM. Results demonstrate that high resolution in all dimensions can be achieved using a relatively short experimental time period (19 h), even though the spectrum is highly congested in the direct and all three indirect dimensions. The combined use of isotags, constant-time pulse sequences, and FDM permits rapid isolation of sugar ring proton spin systems in multiple dimensions and enables all endocyclic J-couplings to be simply measured, the key goal to assigning sugar stercochemistry and anomeric configuration. A general method for rapid, unambiguous elucidation of spin systems in oligosaccharides has been a long-sought goal of carbohydrate NMR, and isotags combined with the FDM now enable this to be easily performed. Additional general advantages of the FDM program for generating high-resolution 2D slices in any dimension from a 4D spectrum are emphasized. (C) 2004 Elsevier Inc. All rights reserved.