波谱学杂志 ›› 2008, Vol. 25 ›› Issue (3): 297-306.

• 研究论文 •    下一篇

基于WATERGATE的双溶剂峰抑制方法

周志明1,2; 张许1; 蒋宾1,2; 夏圣安1,2; 蓝文贤1,2; 李雪1,2; 叶朝辉1; 刘买利1*   

  1. [1.波谱与原子分子物理国家重点实验室(中国科学院 武汉物理与数学研究所),湖北 武汉 430071; 2.中国科学院 研究生院,北京 100049]
  • 收稿日期:2007-11-19 修回日期:2007-12-10 出版日期:2008-09-05 发布日期:2009-12-05
  • 通讯作者: 刘买利

Extending WATERGATE for Suppression of Binary Solvent Signals in NMR Spectroscopy

ZHOU Zhi-ming1,2; ZHANG Xu1; JIANG Bin1,2; XIA Sheng-an1,2; LAN Wen-xian1,2; LI Xue1,2; YE Chao-hui1; LIU Mai-li1*
  

  1. [1.State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics (Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, Wuhan 430071, China); 2.Graduate School of Chinese Academy of Sciences, Beijing 100039, China]
  • Received:2007-11-19 Revised:2007-12-10 Online:2008-09-05 Published:2009-12-05
  • Contact: Liu Mai-li

摘要: WATERGATE(W3/W5)是NMR实验中使用较为广泛的溶剂峰抑制方法,但该方法通常仅能对一个溶剂信号进行有效抑制. 本文对WATERGATE的脉冲序列进行修饰、优化,发展了两种新的双溶剂峰抑制方法. 实验结果表明,经过修饰、优化后的WATERGATE,实验的设立非常简单,不需要复杂的优化过程就能够对双(多)溶剂峰进行有效抑制, 可用于常规1D & 2D NMR 实验、HPLC NMR实验,以及天然产物粗提取物的分析中.

关键词: NMR, 双溶剂峰抑制, WATERGATE, HPLC NMR, 天然产物分析

Abstract: Solvent signal suppression is essential for biological NMR spectroscopy. For applications using reversed-phase HPLC-NMR or studies of natural product extracts with mixed solvents, simultaneous suppression of the signals from multiple solvents is often required in order to get high quality NMR spectrum. There are a number of approaches developed for solvent signal suppression. Although most of these approaches can be used for multiple solvent signals suppression, simple methods with high suppression efficiency are still needed. In this article, double WATERGATE approach was extended for such purpose. Two simple extensions, DSSW5 (Double Solvent Suppression WATERGATE) and GASP-W5 (GASP-based WATERGATE), were established and used to acquire one- and two-dimensional (1D & 2D) NMR spectra in HPLC-NMR and from natural product extracts, respectively. The results demonstrated that the new methods are easy to implement and applicable for routine NMR spectroscopy.

Key words: NMR, solvent signal suppression, WATERGATE, HPLC-NMR, natural product analysis

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