Implementation of real-time two-dimensional nuclear magnetic resonance spectroscopy for on-flow high-performance liquid chromatography

被引:7
作者
Zhou, Zhiming
Lan, Wenxian
Zhang, Weinong
Zhang, Xu
Xia, Sheng'an
Zhu, Hang
Ye, Chaohui
Liu, Maili [1 ]
机构
[1] Chinese Acad Sci, Wuhan Inst Phys & Math, State Key Lab Magnet Resonance & Atom & Mol Phys, Wuhan 430071, Peoples R China
[2] Polytech Univ, Coll Food Sci & Engn, Wuhan 430023, Peoples R China
[3] Chinese Acad Sci, Grad Sch, Beijing 100039, Peoples R China
基金
中国国家自然科学基金;
关键词
HPLC; NMR; HPLC-2D-NMR; Hadamard; amino acids; urine;
D O I
10.1016/j.chroma.2007.04.018
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Directly coupled HPLC-NMR has become a powerful tool for separation and structural elucidation of unknown compounds. However, there are only a few reports on application of on-flow two-dimensional (2D) NMR in HPLC-NMR. Here we present an alternative method for recording realtime 2D-NMR spectrum (total correlation spectroscopy, TOCSY) on a commercial HPLC-NMR system. The method is based on well-established Hadamard matrix for 2D-NMR frequency encoding. In addition, a modified/improved solvent suppression approach is incorporated. This makes it possible to carry out the experiment with both polar and gradient eluents, the widely used chromatographic conditions. The method is exampled using a synthesized mixture of three amino acids (His, Phe and Try) and a human urine sample. The method demonstrated here may be utilized for high-throughput structural or unknown component identification and fast dynamic study in a variety of applications. (c) 2007 Elsevier B.V. All rights reserved.
引用
收藏
页码:464 / 468
页数:5
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