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Updated: May 19, 2026

A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants
Published on: January 1, 2016
Simple, rapid, and sensitive determination of beta-blockers in environmental water using dispersive liquid-liquid
María del Mar Parrilla Vázquez1, Piedad Parrilla Vázquez, Maria Martínez Galera
1Departamento de Hidrogeología y Química Analítica, Universidad de Almería, Campus de Excelencia Agroalimentario, La Cañada de San Urbano, Almería, Spain. parrilla@ual.es
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.
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