title: Determination of five beta-blockers in wastewaters by coupled-column liquid chromatography and fluorescence detection.
abstract: A simple multidimensional system for direct injection of large volumes has been developed for the determination of five beta-blockers (atenolol, nadolol, metoprolol, bisoprolol and betaxolol) in wastewater using fluorescence detection. A C18 50 mm x 4.6 mm i.d. column coupled to a RP Amide C16 150 mm x 4.6 mm i.d. column for analyte clean-up and determination were used, respectively. The capability of a first column for eliminating large, interfering molecules, combined with an optimised, coupled-column liquid chromatography separation procedure (LC-LC), large volume injection (LVI) and fluorescence detection (FD), gave excellent sensitivity and selectivity for the target analytes. The LVI-LC-LC-FD method combines analyte isolation, preconcentration and determination into a single step. Detection limits obtained in wastewater were lower than, or equal to, 0.0020 microg L(-1). Limits of quantification (LOQs) obtained in the matrix according to IUPAC, ranged between 0.0052 and 0.0089 microg L(-1), whereas LOQs calculated according to EURACHEM Guidance, varied between 0.4 and 0.6 microg L(-1). Accuracy values ranged from 82 to 107% (n=3) and relative standard deviation (RSD) values ranged from 0.8 to 9%. The LVI-LC-LC-FD method was applied for determining the target analytes in wastewater samples obtained in Almería (Spain).
authors.affiliation: Department of Analytical Chemistry, University of Almería, La Cañada de San Urbano, 04120 Almería, Spain. parrilla@ual.es
authors.forename: P
authors.initials: P
authors.lastname: Parrilla Vázquez
authors.forename: M
authors.initials: M
authors.lastname: Martínez Galera
authors.forename: A
authors.initials: A
authors.lastname: Serrano Guirado
authors.forename: M M
authors.initials: MM
authors.lastname: Parrilla Vázquez
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000032:analysis* / Q000302:isolation & purification; D053000:Analytic Sample Preparation Methods; D002853:Chromatography, Liquid / Q000191:economics / Q000379:methods*; D007267:Injections; D009930:Organic Chemicals / Q000737:chemistry; D015203:Reproducibility of Results; D012449:Safety; D012997:Solvents / Q000737:chemistry; D013050:Spectrometry, Fluorescence / Q000191:economics / Q000379:methods*; D013997:Time Factors; D014865:Waste Disposal, Fluid; D014867:Water / Q000737:chemistry*
chemical_list: D000319:Adrenergic beta-Antagonists; D009930:Organic Chemicals; D012997:Solvents; D014867:Water