A comparison of capillary-scale LC-NMR with alternative techniques: spectroscopic and practical considerations

被引：27

作者：

Lewis, RJ ^{[1
]}

Bernstein, MA ^{[1
]}

Duncan, SJ ^{[1
]}

Sleigh, CJ ^{[1
]}

机构：

[1] AstraZeneca R&D Charnwood, Dept Phys & Metab Sci, Loughborough LE11 5RH, Leics, England

来源：

MAGNETIC RESONANCE IN CHEMISTRY | 2005年 / 43卷 / 09期

关键词：

NMR; H-1; LC-NMR; capillary LC; cryoprobe; solid-phase extraction; off-line purification; metabolite identification;

D O I：

10.1002/mrc.1614

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

Experimental and practical details for the use of capillary LC (CapLC)-NMR are reported. The capillary NMR probe has high sensitivity and excellent flow characteristics and we found CapLC-NMR to be best suited to samples that are truly mass limited. CapLC-NMR relies on good capillary-scale chromatography where highly concentrated peaks with a volume closely matched to the NMR flow cell are achievable. Provided that the loading capacity of the capillary column is not limiting, the combination of high sensitivity and high solvent suppression quality makes CapLC-NMR an excellent choice. For many real samples, however, the loading is limiting and we found the combination of LC-SPE-MS-NMR with a cryoprobe enables more material to be purified for NMR analysis, while retaining sensitivity. Copyright (c) 2005 John Wiley & Sons, Ltd.

引用

页码：783 / 789

页数：7

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