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Science 22 December 1995:
Vol. 270. no. 5244, pp. 1967 - 1970
DOI: 10.1126/science.270.5244.1967
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Reports

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

Dean L. Olson,  Timothy L. Peck,  Andrew G. Webb,  Richard L. Magin,  Jonathan V. Sweedler (1)

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


D. L. Olson and J. V. Sweedler, Beckman Institute and Department of Chemistry, University of Illinois, 600 S. Mathews, Urbana, IL 61801, USA.
T. L. Peck, A. G. Webb, R. L. Magin, Magnetic Resonance Engineering Laboratory, Beckman Institute, and Department of Electrical and Computer Engineering, University of Illinois, 405 N. Mathews, Urbana, IL 61801, USA.
(1) To whom correspondence should be addressed.


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