Investigation of the feasibility of directly-coupled HPLC-NMR with super(2)H detection with application to the metabolism of N-dimethylformamide-d sub(7)

The use of super(2)H NMR spectroscopy as a detector for HPLC has been investigated using the continuous flow method in which rat urine containing metabolites of N-dimethylformamide-d sub(7) was employed as a test case. Three xenobioticrelated species, including DMF-d sub(7) itself, were detected. It...

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Bibliographic Details
Published in:Journal of pharmaceutical and biomedical analysis 1997-09, Vol.16 (1), p.1-5
Main Authors: Farrant, R D, Cupid, B C, Nicholson, J K, Lindon, J C
Format: Article
Language:English
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Summary:The use of super(2)H NMR spectroscopy as a detector for HPLC has been investigated using the continuous flow method in which rat urine containing metabolites of N-dimethylformamide-d sub(7) was employed as a test case. Three xenobioticrelated species, including DMF-d sub(7) itself, were detected. It is shown that for small molecules which give relatively sharp super(2)H NMR resonances, super(2)H 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 super(2)H-labelled xenobiotics to determine HPLC retention times of metabolites with continuous-flow super(2)H NMR spectroscopy detection, followed by stop-flow super(1)H HPLC-NMR spectroscopy for structural characterisation.
ISSN:0731-7085