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Titolo:
Enantiomeric separation of metoprolol and alpha-hydroxymetoprolol by liquid chromatography and fluorescence detection using a chiral stationary phase
Autore:
Mistry, B; Leslie, JL; Eddington, ND;
Indirizzi:
Univ Maryland, Sch Pharm, Dept Pharmaceut Sci, Baltimore, MD 21201 USA Univ Maryland Baltimore MD USA 21201 rmaceut Sci, Baltimore, MD 21201 USA
Titolo Testata:
JOURNAL OF CHROMATOGRAPHY B
fascicolo: 2, volume: 758, anno: 2001,
pagine: 153 - 161
SICI:
1387-2273(20010715)758:2<153:ESOMAA>2.0.ZU;2-T
Fonte:
ISI
Lingua:
ENG
Soggetto:
HUMAN-PLASMA; URINE; COLUMN; METABOLITES; ASSAY;
Keywords:
enantiomer separation; chiral stationary phases; LC; metoprolol; alpha-hydroxymetoprolol;
Tipo documento:
Article
Natura:
Periodico
Settore Disciplinare:
Life Sciences
Citazioni:
22
Recensione:
Indirizzi per estratti:
Indirizzo: Eddington, ND Univ Maryland, Sch Pharm, Dept Pharmaceut Sci, 100 Penn St,AHB, Baltimore,MD 21201 USA Univ Maryland 100 Penn St,AHB Baltimore MD USA 21201 201 USA
Citazione:
B. Mistry et al., "Enantiomeric separation of metoprolol and alpha-hydroxymetoprolol by liquid chromatography and fluorescence detection using a chiral stationary phase", J CHROMAT B, 758(2), 2001, pp. 153-161

Abstract

A sensitive and stereoselective high-performance liquid chromatographic assay for the determination of the enantiomers of metoprolol (R- and S-) and the diastereoisomers of alpha -hydroxymetoprolol (IIA, IIB) in plasma is reported. Chromatography involved direct separation of enantiomers using a Chirobiotic T bonded phase column (250x4.6 mm) and a mobile phase consisting of acetonitrile-methanol-methylene chloride-glacial acetic acid-triethylamine (56:30:14:2:2, v/v). Solid-phase extraction using silica bonded with ethyl group (C,) was used to extract the compounds of interest from plasma andatenolol was used as the internal standard. The column effluent was monitored using fluorescence detection with excitation and emission wavelengths of 225 and 310 nm, respectively. S-Metoprolol, R-metoprolol, IIB and IIA eluted at about 5.9, 6.7, 7.3 and 8.2 min without any interfering peaks. The calibration curve was linear over the ranger of 0.5 to 100 ng/ml for each isomer of metoprolol acid 1 to 100 ng/ml for each isomer of alpha -hydroxymetoprolol (IIA & IIB). The mean intra-run accuracies were in the range of 96.2 to 114% for R-metoprolol, 94.0 to 111% for S-metoprolol, 90.2 to 110% forIIA, and 94.6 to 106% for IIB. The mean intra-run precisions were all in the range of 2.2 to 12.0% for R-metoprolol, 2.1 to 11.1% for S-metoprolol, 1.9 to 14.5% for IIA, and 3.2 to 11.0% for IIB. The lowest level of quantitation for the enantiomers of metoprolol was 0.5 ng/ml and 1.0 ng/ml for alpha -hydroxymetoprolol (IIA and IIB). The absolute recoveries for each analyte was greater than or equal to 95%. The validated method accurately quantitated the enantiomers of parent drug and metabolite after a single dose of an extended release metoprolol formulation. (C) 2001 Elsevier Science B.V. All rights reserved.

ASDD Area Sistemi Dipartimentali e Documentali, Università di Bologna, Catalogo delle riviste ed altri periodici
Documento generato il 26/01/20 alle ore 10:14:18