Improved spin-echo-edited NMR diffusion measurements

被引:38
作者
Otto, WH [1 ]
Larive, CK [1 ]
机构
[1] Univ Kansas, Dept Chem, Lawrence, KS 66045 USA
关键词
NMR; mixture analysis; diffusion; spin echo;
D O I
10.1006/jmre.2001.2444
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
The need for simple and robust schemes for the analysis of ligand- protein binding has resulted in the development of diffusion-based NMR techniques that can be used to assay binding in protein solutions containing a mixture of several ligands. As a means of gaining spectral selectivity in NMR diffusion measurements, a simple experiment, the gradient modified spin-echo (GOSE), has been developed to reject the resonances of coupled spins and detect only the singlets in the H-1 NMR spectrum. This is accomplished by first using a spin echo to null the resonances of the coupled spins. Following the spin echo, the singlet magnetization is flipped out of the transverse plane and a dephasing gradient is applied to reduce the spectral artifacts resulting from incomplete cancellation of the J-coupled resonances. The resulting modular sequence is combined here with the BPPSTE pulse sequence; however, it could be easily incorporated into any pulse sequence where additional spectral selectivity is desired. Results obtained with the GOSE-BPPSTE pulse sequence are compared with those obtained with the BPPSTE and CPMG-BPPSTE experiments for a mixture containing the ligands resorcinol and tryptophan in a solution of human serum albumin. (C) 2001 Elsevier Science.
引用
收藏
页码:273 / 276
页数:4
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