Investigation of the feasibility of directly-coupled HPLC-NMR with 2H detection with application to the metabolism of N-dimethylformamide-d7

Journal of Pharmaceutical and Biomedical Analysis
R D FarrantJ C Lindon

Abstract

The use of 2H NMR spectroscopy as a detector for HPLC has been investigated using the continuous flow method in which rat urine containing metabolites of N-dimethylformamide-d7 was employed as a test case. Three xenobiotic-related species, including DMF-d7 itself, were detected. It is shown that for small molecules which give relatively sharp 2H NMR resonances, 2H HPLC-NMR spectroscopy is a feasible technique. For larger molecules, the resulting broad lines are likely to preclude the determination of detailed structural information. However, extension of the approach is possible by the use of selectively 2H-labelled xenobiotics to determine HPLC retention times of metabolites with continuous-flow 2H NMR spectroscopy detection, followed by stop-flow 1H HPLC-NMR spectroscopy for structural characterisation.

References

Jan 1, 1989·Journal of Pharmaceutical and Biomedical Analysis·K TulipJ A Timbrell
Aug 1, 1993·Journal of Pharmaceutical and Biomedical Analysis·R D FarrantJ K Nicholson
Oct 1, 1993·Journal of Pharmaceutical and Biomedical Analysis·M SpraulJ C Lindon

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Citations

Feb 27, 1999·Current Opinion in Biotechnology·P A Keifer
Jan 20, 2006·Journal of Zhejiang University. Science. B·Yong Liu, Ling Yang
Nov 25, 2000·Journal of Chromatography. B, Biomedical Sciences and Applications·J C LindonI D Wilson

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