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Liquid chromatography-thermospray tandem mass spectrometry for identification of a heptabarbital metabolite and sample work-up artefacts

Authors
Journal
Journal of Chromatography A
0021-9673
Publisher
Elsevier
Publication Date
Volume
554
Identifiers
DOI: 10.1016/s0021-9673(01)88450-8

Abstract

Abstract An unknown heptabarbital metabolite, observed in the liquid chromatogram of rat plasma and urine samples after administration of heptabarbital, was identified by liquid chromatography-thermospray tandem mass spectrometry. By applying the parent scan mode for screening and the daughter scan mode for structure elucidation, the metabolite was determined to be 5-ethyl-5-(1′-3′- or 6′-cycloheptadienyl)barbituric acid. It was demonstrated that artefact formation occurred when hydrochloric acid was used for conjugate hydrolysis in the sample clean-up. Identification of the artefacts was achieved by the same method. Confirmation of the structures of the metabolite and the artefacts was obtained by gas chromatography-electron impact mass spectrometry.

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