NMR diffusion measurements in complex mixtures using constant-time-HSQC-IDOSY and computer-optimized spectral aliasing for high resolution in the carbon dimension.
NMR diffusion measurements in complex mixtures using constant-time-HSQC-IDOSY and computer-optimized spectral aliasing for high resolution in the carbon dimension.
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DOI：
10.1021/ac060744g
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发表时间：
2006-07
影响因子：
7.4
通讯作者：
B. Vitorge;D. Jeannerat
中科院分区：
文献类型：
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作者：
B. Vitorge;D. Jeannerat
提出了一种新的用于复杂混合物核磁共振扩散测量的三维脉冲序列。该方法基于恒时间（CT） HSQC实验，将扩散延迟与碳析出时间相结合。这种组合在碳维度上具有获得高分辨率的巨大潜力。当使用碳维度的经典采样时，最大分辨率将需要大量的时间增量，从而导致不切实际的长采集时间。计算机优化的光谱混叠技术的应用，可以利用一维碳光谱、HSQC实验或两者的信息含量，将时间增量的数量和总采集时间减少1-2个数量级。通过新的CT-HSQC-IDOSY实验，在0.1 M D2O的葡萄糖、麦芽糖和麦芽糖溶液中，存在的6种异头物在8 h内可以得到自然丰度的扩散速率，标准偏差小于5%。
A new 3D pulse sequence for NMR diffusion measurements in complex mixtures is presented. It is based on the constant-time (CT) HSQC experiment and combines diffusion delay with the carbon evolution time. This combination has great potential to obtain high resolution in the carbon dimension. When using classical sampling of the carbon dimension, maximal resolution would require a large number of time increments, leading to unrealistically long acquisition times. The application of computer-optimized spectral aliasing allows one to reduce the number of time increments and the total acquisition time by 1-2 orders of magnitude by taking advantage of the information content of 1D carbon spectra, HSQC experiments, or both. With the new CT-HSQC-IDOSY experiment, the diffusion rates of the six anomers present in a 0.1 M D2O solution of glucose, maltose, and maltotriose could be obtained at natural abundance in 8 h with standard deviations below 5%.