title: Determination of narciclasine in serum by reversed-phase high-performance liquid chromatography: comparison of amperometric, ultraviolet photometric and fluorescence detection.
abstract: Narciclasine was determined in the blood of mice by reversed-phase high-performance liquid chromatography, using a C18 stationary phase and a mobile phase of methanol-0.025 M potassium dihydrogen phosphate (50:50, v/v) of pH 5.5. Amperometric detection at a carbon fibre array working electrode held at +1.8 V (Ag/AgCl) permitted determination down to concentrations of 10 and 15.4 ng ml-1 (at a signal-to-noise ratio of 2) in aqueous solution and in serum, respectively. Fluorescence detection (excitation and emission wavelengths of 360 and 480 nm, respectively) exhibited somewhat poorer sensitivities for aqueous and serum samples: the respective limits of detection were 25 and 32 ng ml-1 at a signal-to-noise ratio of 2. Both the amperometric and the fluorescence detection were free from interference from blood components, but the fluorescence measurement required a post-column pH adjustment. UV photometric detection at 254 nm exhibited detection limits of 15 and 65 ng ml-1 in aqueous samples and in serum, respectively, and suffered from interferences from blood components that strongly absorbed in the ultraviolet region. All three detection techniques exhibited good linearity and precision.
authors.affiliation: Department of Analytical Chemistry, Charles University, Prague, Czechoslovakia.
authors.forename: I
authors.initials: I
authors.lastname: Svagrová
authors.forename: K
authors.initials: K
authors.lastname: Stulík
authors.forename: V
authors.initials: V
authors.lastname: Pacáková
authors.forename: P
authors.initials: P
authors.lastname: Caliceti
authors.forename: F M
authors.initials: FM
authors.lastname: Veronese
mesh_terms: D000470:Alkaloids / Q000097:blood*; D047151:Amaryllidaceae Alkaloids; D000818:Animals; D000970:Antineoplastic Agents / Q000097:blood; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004563:Electrochemistry / Q000379:methods; D007202:Indicators and Reagents; D051379:Mice; D008815:Mice, Inbred Strains; D010617:Phenanthridines; D013050:Spectrometry, Fluorescence / Q000379:methods; D013056:Spectrophotometry, Ultraviolet / Q000379:methods
chemical_list: D000470:Alkaloids; D047151:Amaryllidaceae Alkaloids; D000970:Antineoplastic Agents; D007202:Indicators and Reagents; D010617:Phenanthridines; C010753:narciclasine