Leiden University Scholarly Publications

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Wouters, B.; Miggiels, A.L.W.; Bezemer, R.P.; Cruijsen, E.A.W. van der; Leeuwen, E. van; Gauvin, J.; ... ; Hankemeier, T. (2022)

Automated segmented-flow analysis: NMR with a novel fluoropolymer flow cell for high-throughput screening

Article / Letter to editor
High-throughput analysis in fields such as industrial biotechnology, combinatorial chemistry, and life sciences is becoming increasingly important. Nuclear magnetic resonance (NMR) spectroscopy is a powerful technique providing exhaustive molecular information on complex samples. Flow NMR in particular is a cost and time-efficient method for large screenings. In this study, we have developed a novel 3.0 mm inner diameter polychlorotrifluoroethylene (PCTFE) flow cell for a segmented-flow analysis (SFA) - NMR automated platform. The platform uses FC-72 fluorinated oil and fluoropolymer components to achieve a fully fluorinated flow path. Samples were repeatably transferred from 96-deepwell plates to the flow cell by displacing a fixed volume of oil, with a transfer time of 42 s. 1H spectra were acquired fully automated with 500 and 600 MHz NMR spectrometers. The spectral performance of the novel PCTFE cell was equal to that of commercial glass cells. Peak area repeatability was...Show moreHigh-throughput analysis in fields such as industrial biotechnology, combinatorial chemistry, and life sciences is becoming increasingly important. Nuclear magnetic resonance (NMR) spectroscopy is a powerful technique providing exhaustive molecular information on complex samples. Flow NMR in particular is a cost and time-efficient method for large screenings. In this study, we have developed a novel 3.0 mm inner diameter polychlorotrifluoroethylene (PCTFE) flow cell for a segmented-flow analysis (SFA) - NMR automated platform. The platform uses FC-72 fluorinated oil and fluoropolymer components to achieve a fully fluorinated flow path. Samples were repeatably transferred from 96-deepwell plates to the flow cell by displacing a fixed volume of oil, with a transfer time of 42 s. 1H spectra were acquired fully automated with 500 and 600 MHz NMR spectrometers. The spectral performance of the novel PCTFE cell was equal to that of commercial glass cells. Peak area repeatability was excellent with a relative standard deviation of 0.1-0.5% for standard samples, and carryover was below 0.2% without intermediate washing. The sample temperature was conditioned by using a thermostated transfer line in order to reduce the equilibration time in the probe and increase the throughput. Finally, analysis of urine samples demonstrated the applicability of this platform for screening complex matrices.Show less
All authors
Wouters, B.; Miggiels, A.L.W.; Bezemer, R.P.; Cruijsen, E.A.W. van der; Leeuwen, E. van; Gauvin, J.; Houben, K.; Sai Sankar Gupta, K.B.; Zuijdwijk, P.; Harms, A.C.; Carvalho de Souza, A.; Hankemeier, T.
Date
2022-10-27
Journal
Analytical Chemistry
Volume
94
Issue
44
Pages
15350 - 15358
DOI
doi:10.1021/acs.analchem.2c03038