title: Achiral and chiral high-performance liquid chromatography of verapamil and its metabolites in serum samples.
abstract: Rapid and simple achiral and chiral HPLC assays have been developed for the determination of verapamil and its metabolites in serum samples. Two achiral reversed-phase columns, Hisep C18 (150 x 4.6 mm) and NovaPak C18 (150 x 3.9 mm) were used for the simultaneous separation of all analyzed compounds. An alpha1-AGP column (100 x 4.0 mm) was recommended for successful chiral separations of verapamil and its seven metabolites. All analyses were realised with fluorescence detection at lambda(ex) = 276 nm and lambda(em) = 310 nm. Limits of quantitation were in the range 1.0 to 5 ng/ml for all compounds. Both off-line SPE (SepPak C18 cartridges) and the on-line SPE with a semipermeable surface SDS C8 pre-column, (10 x 4.6 mm) were used for the clean-up and sample preconcentration. Extraction recoveries for all analyzed compounds were 87.7 +/- 5.8 to 92.7 +/- 4.0% for off-line SPE and 94.3 +/- 4.2 to 98.2 +/- 5.1% for on-line SPE. The complete assay could be applied for achiral and chiral monitoring verapamil and all its metabolites in serum samples.
authors.affiliation: Faculty of Chemical Technology, Department of Analytical Chemistry, Slovak Technical University, Bratislava, Slovak Republic.
authors.forename: E
authors.initials: E
authors.lastname: Brandsteterová
authors.forename: I W
authors.initials: IW
authors.lastname: Wainer
mesh_terms: D002121:Calcium Channel Blockers / Q000097:blood* / Q000378:metabolism; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D011786:Quality Control; D015203:Reproducibility of Results; D014700:Verapamil / Q000097:blood* / Q000378:metabolism
chemical_list: D002121:Calcium Channel Blockers; D014700:Verapamil