title: Simple, rapid, and sensitive determination of beta-blockers in environmental water using dispersive liquid-liquid microextraction followed by liquid chromatography with fluorescence detection.
abstract: A novel method, dispersive liquid-liquid microextraction combined with liquid chromatography-fluorescence detection is proposed for the determination of three beta-blockers (metoprolol, bisoprolol, and betaxolol) in ground water, river water, and bottled mineral water. Some important parameters, such as the kind and volume of extraction and dispersive solvents, extraction time, pH, and salt effect were investigated and optimized. In the method, a suitable mixture of extraction solvent (60 μL carbon tetrachloride) and dispersive solvent (1 mL acetonitrile) were injected into the aqueous samples (5.00 mL) and the cloudy solution was observed. After centrifugation, the enriched analytes in the bottom CCl(4)  phase were determined by liquid chromatography with fluorescence detection. Under the optimum conditions, the enrichment factors (EFs) for metoprolol, bisoprolol, and betaxolol were 180, 190, and 182, and the limits of detection (LODs) were 1.8, 1.4, and 1.0 ng L(-1) , respectively. A good linear relationship between the peak area and the concentration of analytes was obtained in the range of 3-150 ng L(-1) . The relative standard deviations (RSDs) for the extraction of 10 ng L(-1)  of beta-blockers were in the range of 4.6-5.7% (n = 5). Compared with other methods, dispersive liquid-liquid microextraction is a very simple, rapid, sensitive (low limit of detection), and economical (only 1.06 mL volume of organic solvent) method, which is in compliance with the requirements of green analytical methodologies.
authors.affiliation: Departamento de Hidrogeología y Química Analítica, Universidad de Almería, Campus de Excelencia Agroalimentario, La Cañada de San Urbano, Almería, Spain. parrilla@ual.es
authors.forename: María del Mar
authors.initials: Mdel M
authors.lastname: Parrilla Vázquez
authors.forename: Piedad
authors.initials: P
authors.lastname: Parrilla Vázquez
authors.forename: Maria
authors.initials: M
authors.lastname: Martínez Galera
authors.forename: Luis
authors.initials: L
authors.lastname: Molina Sánchez
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000032:analysis* / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D059627:Liquid Phase Microextraction / Q000379:methods*; D012680:Sensitivity and Specificity; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification*; D014877:Water Pollution, Chemical / Q000032:analysis
chemical_list: D000319:Adrenergic beta-Antagonists; D014874:Water Pollutants, Chemical