Fluorescence detection of cardenolides in reversed-phase high-performance liquid chromatography after post-column derivatization |
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| Affiliation: | 1. Department of Psychiatry, Leiden University Medical Center, Leiden, The Netherlands;2. Department of Psychiatry, CAPRI-University of Antwerp, Antwerp, Belgium;3. Department of Psychiatry, Haga Ziekenhuis, The Hague, The Netherlands;4. Department of Clinical Chemistry, Endocrine Laboratory, VU University Medical Center, Amsterdam, The Netherlands;5. Department of Public Health and Primary Care, Leiden University Medical Center, Leiden, The Netherlands;6. GGZ InGeest, Department of Psychiatry, EMGO Institute for Health and Care Research, VU University Medical Center, Amsterdam, The Netherlands;1. Laboratory of Cardiovascular Pharmacology, Faculty of Medical Sciences and Teaching Hospital, University of Campinas (Unicamp), Campinas, SP, Brazil;2. Faculty of Medicine, Pontifical Catholic University of Campinas (Puccamp), Campinas, SP, Brazil |
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| Abstract: | Methods for the fluorescence derivatization of cardiac glycosides with concentrated acids from TLC are adopted to HPLC for post-column derivatization. The column effluent is blended with concentrated acids in a knitted tube reactor, which enables derivatization with negligible increase in chromatographic peak width. The selectivity of the reaction is temperature-dependent and influenced by the respective acid. Reactivity increases from H3PO4→CH3SO3H ≡ H2SO4. The conversion of digoxigenin, digitoxigenin and their digitoxosides is accelerated by Cu(II) acetate or Co(II) nitrate in H2SO4. Combined with a new two-mode, single-column solid-phase sample preparation, cardiac glycoside levels of less than 100 pg/glycoside in 1 ml plasma are detectable. |
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