Quantitative 2D HSQC (Q-HSQC) via suppression of J-dependence of polarization transfer in NMR spectroscopy:: Application to wood lignin

被引:230
作者
Heikkinen, S [1 ]
Toikka, MM [1 ]
Karhunen, PT [1 ]
Kilpeläinen, IA [1 ]
机构
[1] Univ Helsinki, Inst Biotechnol, NMR Lab, FIN-00014 Helsinki, Finland
关键词
D O I
10.1021/ja029035k
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
A quantitative method to record H-1-C-13 correlation NMR spectra (Q-HSQC) is presented. The suppression Of (1)J(CH)-dependence is achieved by modulating the polarization transfer delays of HSQC. In addition, the effect of homonuclear couplings, as well as relaxation during the pulse sequence are discussed. We developed the Q-HSQC approach for the quantitative analysis of wood lignin, a complex polymer where it has been difficult to obtain reliable data on the relative amounts of different structural units. The current method is applicable to a variety of complex mixtures, where normal 1D H-1- and C-13-NMR methods fail.
引用
收藏
页码:4362 / 4367
页数:6
相关论文
共 18 条
[1]   LIGNIN CHEMISTRY - PAST, PRESENT AND FUTURE [J].
ADLER, E .
WOOD SCIENCE AND TECHNOLOGY, 1977, 11 (03) :169-218
[2]   Identification of side-chain structures in a poplar lignin using three-dimensional HMQC-HOHAHA NMR spectroscopy [J].
Ämmälahti, E ;
Brunow, G ;
Bardet, M ;
Robert, D ;
Kilpeläinen, I .
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1998, 46 (12) :5113-5117
[3]  
BAILEY CW, 1969, TAPPI, V52, P491
[4]  
Bjorkman A., 1956, SVEN PAPPERSTIDN, V59, P477, DOI DOI 10.1016/J.CHROMA.2003.08.046
[5]   OXYZIMTALKOHOLE UND IHRE DEHYDRIERUNGS-POLYMERISATE [J].
FREUDENBERG, K ;
HUBNER, HH .
CHEMISCHE BERICHTE-RECUEIL, 1952, 85 (12) :1181-1191
[6]   Synthesis and crystal structure determination of model compounds for the dibenzodioxocine structure occurring in wood lignins [J].
Karhunen, P ;
Rummakko, P ;
Pajunen, A ;
Brunow, G .
JOURNAL OF THE CHEMICAL SOCIETY-PERKIN TRANSACTIONS 1, 1996, (18) :2303-2308
[7]   DIBENZODIOXOCINS - A NOVEL TYPE OF LINKAGE IN SOFTWOOD LIGNINS [J].
KARHUNEN, P ;
RUMMAKKO, P ;
SIPILA, J ;
BRUNOW, G ;
KILPELAINEN, I .
TETRAHEDRON LETTERS, 1995, 36 (01) :169-170
[8]   QUANTITATIVE C-13 NMR CHARACTERIZATION OF LIGNIN .1. A METHODOLOGY FOR HIGH-PRECISION [J].
LANDUCCI, LL .
HOLZFORSCHUNG, 1985, 39 (06) :355-359
[9]  
LAPIERRE C, 1985, HOLZFORSCHUNG, V39, P367
[10]  
MARION D, 1989, J MAGN RESON, V39, P163