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Continuous Flow 1H and 13C NMR Spectroscopy in Microfluidic Stripline NMR Chips

Author:
Oosthoek-de Vries, Anna Jo, Bart, Jacob, Tiggelaar, Roald M., Janssen, Johannes W. G., van Bentum, P. Jan M., Gardeniers, Han J. G. E., Kentgens, Arno P. M.
Source:
Analytical chemistry 2017 v.89 no.4 pp. 2296-2303
ISSN:
1520-6882
Subject:
geometry, magnetic materials, menthol, nuclear magnetic resonance spectroscopy, quantitative analysis, stable isotopes
Abstract:
Microfluidic stripline NMR technology not only allows for NMR experiments to be performed on small sample volumes in the submicroliter range, but also experiments can easily be performed in continuous flow because of the stripline’s favorable geometry. In this study we demonstrate the possibility of dual-channel operation of a microfluidic stripline NMR setup showing one- and two-dimensional ¹H, ¹³C and heteronuclear NMR experiments under continuous flow. We performed experiments on ethyl crotonate and menthol, using three different types of NMR chips aiming for straightforward microfluidic connectivity. The detection volumes are approximately 150 and 250 nL, while flow rates ranging from 0.5 μL/min to 15 μL/min have been employed. We show that in continuous flow the pulse delay is determined by the replenishment time of the detector volume, if the sample trajectory in the magnet toward NMR detector is long enough to polarize the spin systems. This can considerably speed up quantitative measurement of samples needing signal averaging. So it can be beneficial to perform continuous flow measurements in this setup for analysis of, e.g., reactive, unstable, or mass-limited compounds.
Agid:
5634814