Accurate measurement of long-range heteronuclear coupling constants from undistorted multiplets of an enhanced CPMG-HSQMBC experiment

被引:50
作者
Kövér, KE
Batta, G
Fehér, K
机构
[1] Univ Debrecen, Dept Inorgan & Analyt Chem, H-4010 Debrecen, Hungary
[2] Univ Debrecen, Hungarian Acad Sci, Dept Pharmaceut Chem, H-4010 Debrecen, Hungary
[3] Univ Debrecen, Hungarian Acad Sci, Res Grp Antibiot, H-4010 Debrecen, Hungary
[4] Max Planck Inst Med Res, Dept Biomol Mech, D-69120 Heidelberg, Germany
基金
匈牙利科学研究基金会;
关键词
long-range heteronuclear couplings; HSQMBC; CPMG; composite pulses; carbohydrate; glycopeptide;
D O I
10.1016/j.jmr.2006.03.015
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Here, we present a modified CPMG-HSQMBC experiment which is capable to reduce the detrimental phase twists in the "longrange" connectivity multiplets caused by proton-proton couplings. We demonstrate that concerted CPMG pulse trains applied on both nuclei in the starting CPMG-INEPT transfer step can considerably be improved by composite pi pulses that compensate for pulse imperfections and off-resonance effects. Experimental optimization of the interpulse delay within the CPMG cycle was found to be crucial in order to achieve the best possible "decoupling" of homonuclear coupling modulation. (c) 2006 Elsevier Inc. All rights reserved.
引用
收藏
页码:89 / 97
页数:9
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