High-resolution microcoil NMR for analysis of mass-limited, nanoliter samples.

作者: Dean L. Olson , Michael E. Lacey , Jonathan V. Sweedler

DOI: 10.1021/AC970972Y

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摘要: An improved nanoliter-volume NMR probe design places the microcoil and capillary at magic angle (54.7°) with respect to external magnetic field. Using an which requires a total sample volume of just 200 nL, high-resolution 300-MHz 1H-NMR spectra (line width, 0.6 Hz) are presented 10 mM α-bag cell peptide for observe quantity 45 ng (50 pmol in 5 nL). For inside (the volume, Vobs), 3σ limit detection (LOD) is 9 (10 pmol, 2 mM) data obtained 15 h. To reduce acquisition time, greater Vobs developed. As example rapid, mass-limited analysis, concentration corresponding 400 menthol dissolved = 31 nL (82.6 yields spectrum min (LOD 6.9 ng, 44 1.4 mM). illustrate improvements sensitivity, acquired (12.8 Compared commercial nanoprobe th...

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