TY - JOUR
T1 - High-Resolution Microcoil NMR for Analysis of Mass-Limited, Nanoliter Samples
AU - Olson, Dean
AU - Lacey, Michael E.
AU - Sweedler, Jonathan V
PY - 1998/2/1
Y1 - 1998/2/1
N2 - An improved nanoliter-volume NMR probe design places the microcoil and capillary at the magic angle (54.7°) with respect to the external magnetic field. Using an NMR probe which requires a total sample volume of just 200 nL, high-resolution 300-MHz 1H-NMR spectra (line width, 0.6 Hz) are presented of 10 mM α-bag cell peptide for an observe quantity of 45 ng (50 pmol in 5 nL). For the volume of sample inside the microcoil (the observe volume, Vobs), the 3σ limit of detection (LOD) is 9 ng (10 pmol, 2 mM) for data obtained in 15 h. To reduce the data acquisition time, a probe with a greater Vobs is developed. As an example of a rapid, mass-limited analysis, a concentration corresponding to 400 ng of menthol dissolved in Vobs = 31 nL (82.6 mM) yields a spectrum in 9 min (LOD = 6.9 ng, 44 pmol, 1.4 mM). To illustrate improvements in concentration sensitivity, a spectrum is acquired in 45 min for 400 ng of menthol dissolved in a total sample volume of 200 nL (12.8 mM). Compared to a commercial nanoprobe for the same mass of menthol, these two examples reduce data acquisition time by at least 95%. Both model compounds demonstrate substantially improved concentration LODs compared to those obtained hi previous high-resolution, microcoil NMR work. These advances illustrate the utility of enhanced sensitivity provided by NMR microcoils applied to nanoliter volumes of mass-limited samples.
AB - An improved nanoliter-volume NMR probe design places the microcoil and capillary at the magic angle (54.7°) with respect to the external magnetic field. Using an NMR probe which requires a total sample volume of just 200 nL, high-resolution 300-MHz 1H-NMR spectra (line width, 0.6 Hz) are presented of 10 mM α-bag cell peptide for an observe quantity of 45 ng (50 pmol in 5 nL). For the volume of sample inside the microcoil (the observe volume, Vobs), the 3σ limit of detection (LOD) is 9 ng (10 pmol, 2 mM) for data obtained in 15 h. To reduce the data acquisition time, a probe with a greater Vobs is developed. As an example of a rapid, mass-limited analysis, a concentration corresponding to 400 ng of menthol dissolved in Vobs = 31 nL (82.6 mM) yields a spectrum in 9 min (LOD = 6.9 ng, 44 pmol, 1.4 mM). To illustrate improvements in concentration sensitivity, a spectrum is acquired in 45 min for 400 ng of menthol dissolved in a total sample volume of 200 nL (12.8 mM). Compared to a commercial nanoprobe for the same mass of menthol, these two examples reduce data acquisition time by at least 95%. Both model compounds demonstrate substantially improved concentration LODs compared to those obtained hi previous high-resolution, microcoil NMR work. These advances illustrate the utility of enhanced sensitivity provided by NMR microcoils applied to nanoliter volumes of mass-limited samples.
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U2 - 10.1021/ac970972y
DO - 10.1021/ac970972y
M3 - Article
C2 - 9470492
AN - SCOPUS:0031989836
SN - 0003-2700
VL - 70
SP - 645
EP - 650
JO - Analytical Chemistry
JF - Analytical Chemistry
IS - 3
ER -