title: Comparative validations of non-aqueous capillary electrophoresis and high-performance liquid chromatography methods for the simultaneous determination of histamine H2 receptor antagonists in human urine.
abstract: This paper reports a previously optimised method based on non-aqueous capillary electrophoresis (NACE) using UV detection for the separation and simultaneous determination of cimetidine (CIM), ranitidine (RAN), roxatidine (ROX), nizatidine (NIZ) and famotidine (FAM) in human urine. Separation is performed at 25°C and at a separation voltage of 15kV. Methanol containing 10mM ammonium acetate and 0.2% acetic acid was used as background electrolyte, and detection at 214nm. These conditions allow the five analytes to be separated within 4min. In addition in the present paper a HPLC method using diode-array as well as detector, was proposed as standard analytical method, which chromatography conditions were following: a mobile phase consisting of 80:20 20mM phosphate buffer (pH 7.5)/acetonitrile, and using 1mLmin-1as flow rate of the mobile phase. Detection limits were evaluated on the basis of baseline noise and were establishing between 8 and 15μgL-1for NACE and between 16 and 162μgL-1for HPLC. The methods showed good precision with overall intra- and inter-day variations of 0.5-2.0% and 0.7-3.8%, respectively. Finally the proposed methods were successfully applied to the screening determination of the analytes in human urine, with recoveries between 97 and 105%, being able the use as pharmacokinetic data in clinical urine samples.
authors.affiliation: Department of Analytical Chemistry and Food Technology, Faculty of Chemistry, University of Castilla-La Mancha, Ciudad Real, Spain.
authors.forename: Juan José
authors.initials: JJ
authors.lastname: Berzas Nevado
authors.affiliation: Department of Analytical Chemistry and Food Technology, Faculty of Chemistry, University of Castilla-La Mancha, Ciudad Real, Spain.
authors.forename: Gregorio
authors.initials: G
authors.lastname: Castañeda Peñalvo
authors.affiliation: Department of Analytical Chemistry and Food Technology, Faculty of Chemistry, University of Castilla-La Mancha, Ciudad Real, Spain.
authors.forename: Rosa María
authors.initials: RM
authors.lastname: Rodríguez Dorado
authors.affiliation: Department of Analytical Chemistry and Food Technology, Faculty of Pharmacy, University of Castilla-La Mancha, Albacete, Spain. Electronic address: virginia.rrobledo@uclm.es.
authors.forename: Virginia
authors.initials: V
authors.lastname: Rodríguez Robledo