Enantioselective determination of felodipine in human plasma by chiral normal-phase liquid chromatography and electrospray ionisation mass spectrometry

An analytical method was developed for the determination of the enantiomers of felodipine, a dihydropyridine-type calcium antagonist, in human blood plasma. Felodipine was extracted from plasma using toluene as extraction solvent. The enantiomers were separated on a cellulose tris(4-methyl benzoate)...

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Veröffentlicht in:Journal of pharmaceutical and biomedical analysis 2002-01, Vol.27 (3), p.489-495
Hauptverfasser: Lindmark, Bo, Ahnoff, Martin, Persson, Bengt-Arne
Format: Artikel
Sprache:eng
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Zusammenfassung:An analytical method was developed for the determination of the enantiomers of felodipine, a dihydropyridine-type calcium antagonist, in human blood plasma. Felodipine was extracted from plasma using toluene as extraction solvent. The enantiomers were separated on a cellulose tris(4-methyl benzoate) stationary phase (Chiralcel OJ-R) using 2-propanol– iso-hexane (11:89) as mobile phase. Post-column addition of ammonium acetate in ethanol–water (95:5) allowed sensitive detection of the ammonium adduct by electrospray ionisation and selected reaction monitoring. Deuterated felodipine racemate was used as internal standard. Within-run repeatability was determined and a coefficient of variation below 2% was achieved at 22 nmol/l and below 10% at 0.27 nmol/l. Between-day precision was evaluated and a coefficient of variation of 3.6% at 4 nmol/l plasma was obtained. Limit of quantification (LOQ) was set at 0.25 nmol/l (0.10 μg/l). The method proved adequate for pharmacokinetic studies of R- and S-felodipine after oral administration of therapeutic doses of felodipine.
ISSN:0731-7085
1873-264X
DOI:10.1016/S0731-7085(01)00582-9