Rapid 3D NMR using the filter diagonalization method:: application to oligosaccharides derivatized with 13C-labeled acetyl groups

被引:18
作者
Armstrong, GS
Cano, KE
Mandelshtam, VA
Shaka, AJ
Bendiak, B
机构
[1] Univ Colorado, Hlth Sci Ctr, Dept Cell & Dev Biol, Denver, CO 80262 USA
[2] Univ Colorado, Hlth Sci Ctr, Biomol Struct Program, Denver, CO 80262 USA
[3] Univ Calif Irvine, Dept Chem, Irvine, CA 92697 USA
基金
美国国家科学基金会;
关键词
filter diagonalization method; multi-dimensional NMR; constant-time; C-13; labeling; O-acetylation; oligosaccharides;
D O I
10.1016/j.jmr.2004.06.002
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Rapid 3D NMR spectroscopy of oligosaccharides having isotopically labeled acetyl "isotags" was made possible with high resolution in the indirect dimensions using the filter diagonalization method (FDM). A pulse sequence was designed for the optimal correlation of acetyl methyl protons, methyl carbons, and carbonyl carbons. The multi-dimensional nature of the FDM, coupled with the advantages of constant-time evolution periods, resulted in marked improvements over Fourier transform (FT) and mirror-image linear prediction (MI-LP) processing methods. The three methods were directly compared using identical data sets. A highly resolved 3D spectrum was achieved with the FDM using a very short experimental time (28 min). (C) 2004 Elsevier Inc. All rights reserved.
引用
收藏
页码:156 / 163
页数:8
相关论文
共 19 条
[1]   Regularized resolvent transform for direct calculation of 45° projections of 2D J spectra [J].
Armstrong, GS ;
Chen, JH ;
Cano, KE ;
Shaka, A ;
Mandelshtam, VA .
JOURNAL OF MAGNETIC RESONANCE, 2003, 164 (01) :136-144
[2]   ABSORPTION-SPECTRA FROM PHASE-MODULATED SPIN ECHOES [J].
BAX, A ;
MEHLKOPF, AF ;
SMIDT, J .
JOURNAL OF MAGNETIC RESONANCE, 1979, 35 (03) :373-377
[3]   An effective strategy for structural elucidation of oligosaccharides through NMR spectroscopy combined with peracetylation using doubly 13C-labeled acetyl groups [J].
Bendiak, B ;
Fang, TT ;
Jones, DNM .
CANADIAN JOURNAL OF CHEMISTRY-REVUE CANADIENNE DE CHIMIE, 2002, 80 (08) :1032-1050
[4]   Nuclear magnetic resonance spectroscopy of peracetylated oligosaccharides having 13C-labeled carbonyl groups in lieu of permethylation analysis for establishing linkage substitutions of sugars [J].
Bendiak, B .
CARBOHYDRATE RESEARCH, 1999, 315 (3-4) :206-221
[5]   Adjustable, broadband, selective excitation with uniform phase [J].
Cano, KE ;
Smith, MA ;
Shaka, AJ .
JOURNAL OF MAGNETIC RESONANCE, 2002, 155 (01) :131-139
[6]   Ultra-high resolution 3D NMR spectra from limited-size data sets [J].
Chen, JH ;
Nietlispach, D ;
Shaka, AJ ;
Mandelshtam, VA .
JOURNAL OF MAGNETIC RESONANCE, 2004, 169 (02) :215-224
[7]   Progress on the two-dimensional filter diagonalization method. An efficient doubling scheme for two-dimensional constant-time NMR [J].
Chen, JH ;
De Angelis, AA ;
Mandelshtam, VA ;
Shaka, AJ .
JOURNAL OF MAGNETIC RESONANCE, 2003, 162 (01) :74-89
[8]   Regularization of the two-dimensional filter diagonalization method: FDM2K [J].
Chen, JH ;
Mandelshtam, VA ;
Shaka, AJ .
JOURNAL OF MAGNETIC RESONANCE, 2000, 146 (02) :363-368
[9]   NMRPIPE - A MULTIDIMENSIONAL SPECTRAL PROCESSING SYSTEM BASED ON UNIX PIPES [J].
DELAGLIO, F ;
GRZESIEK, S ;
VUISTER, GW ;
ZHU, G ;
PFEIFER, J ;
BAX, A .
JOURNAL OF BIOMOLECULAR NMR, 1995, 6 (03) :277-293
[10]   AXIAL-PEAK ARTIFACTS IN MULTIPULSE NMR EXPERIMENTS [J].
HAMMARSTROM, A ;
OTTING, G .
JOURNAL OF MAGNETIC RESONANCE SERIES A, 1994, 109 (02) :246-249