High-Resolution Microcoil 1H-NMR for Mass-Limited, Nanoliter-Volume Samples

作者: D. L. Olson , T. L. Peck , A. G. Webb , R. L. Magin , J. V. Sweedler

DOI: 10.1126/SCIENCE.270.5244.1967

关键词:

摘要: High-resolution, proton nuclear magnetic resonance (NMR) spectra of 5-nanoliter samples have been obtained with much higher mass sensitivity [signal-to-noise ratio (S/N) per micromole] than traditional methods. Arginine and sucrose show a mean enhancement 130 compared to 278-microliter run in 5-millimeter tube conventional, commercial probe. This can reduce data acquisition time by factor >16,000 or the needed sample about 130. A linewidth 0.6 hertz was achieved on 300-megahertz spectrometer matching susceptibility medium that surrounds detection cell copper coil. For sucrose, limit (defined at S/N = 3) 19 nanograms (56 picomoles) for 1-minute acquisition. technique should prove useful mass-limited use as detector capillary separations.

参考文章(16)
Timothy R. Saarinen, Charles S. Johnson, High-resolution electrophoretic NMR Journal of the American Chemical Society. ,vol. 110, pp. 3332- 3333 ,(1988) , 10.1021/JA00218A071
Nian. Wu, Andrew. Webb, Timothy L. Peck, Jonathan V. Sweedler, On-line NMR detection of amino acids and peptides in microbore LC. Analytical Chemistry. ,vol. 67, pp. 3101- 3107 ,(1995) , 10.1021/AC00114A002
Denise P. Hinton, Charles S. Johnson, Diffusion ordered 2D NMR spectroscopy of phospholipid vesicles: determination of vesicle size distributions The Journal of Physical Chemistry. ,vol. 97, pp. 9064- 9072 ,(1993) , 10.1021/J100137A038
Ole Vorm, Peter Roepstorff, Matthias Mann, None, Improved resolution and very high sensitivity in MALDI TOF of matrix surfaces made by fast evaporation Analytical Chemistry. ,vol. 66, pp. 3281- 3287 ,(1994) , 10.1021/AC00091A044
Mary D. Oates, Bruce R. Cooper, James W. Jorgenson, Quantitative amino acid analysis of individual snail neurons by open tubular liquid chromatography. Analytical Chemistry. ,vol. 62, pp. 1573- 1577 ,(1990) , 10.1021/AC00214A006
R.D. Black, T.A. Early, G.A. Johnson, Performance of a high-temperature superconducting resonator for high-field imaging Journal of Magnetic Resonance, Series A. ,vol. 113, pp. 74- 80 ,(1995) , 10.1006/JMRA.1995.1058
Purnendu K. Dasgupta, Shaorong. Liu, Electroosmosis: A Reliable Fluid Propulsion System for Flow Injection Analysis Analytical Chemistry. ,vol. 66, pp. 1792- 1798 ,(1994) , 10.1021/AC00083A004
L.F Fuks, F.S.C Huang, C.M Carter, W.A Edelstein, P.B Roemer, Susceptibility, lineshape, and shimming in high-resolution NMR Journal of Magnetic Resonance. ,vol. 100, pp. 229- 242 ,(1992) , 10.1016/0022-2364(92)90258-9
Nian Wu, Timothy L. Peck, Andrew G. Webb, Richard L. Magin, Jonathan V. Sweedler, Nanoliter Volume Sample cells for 1H NMR: Application to Online Detection in Capillary Electrophoresis Journal of the American Chemical Society. ,vol. 116, pp. 7929- 7930 ,(1994) , 10.1021/JA00096A073
R. Black, T. Early, P. Roemer, O. Mueller, A Mogro-Campero, L. Turner, G. Johnson, A high-temperature superconducting receiver for nuclear magnetic resonance microscopy Science. ,vol. 259, pp. 793- 795 ,(1993) , 10.1126/SCIENCE.8430331