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Simple, rapid, and sensitive determination of beta‐blockers in environmental water using dispersive liquid–liquid microextraction followed by liquid chromatography with fluorescence detection
Author(s) -
Vázquez Ma del Mar Parrilla,
Vázquez Piedad Parrilla,
Galera Maria Martínez,
Sánchez Luis Molina
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200222
Subject(s) - chromatography , detection limit , chemistry , extraction (chemistry) , high performance liquid chromatography , solvent , bisoprolol , liquid–liquid extraction , analyte , aqueous solution , analytical chemistry (journal) , medicine , heart failure , organic chemistry
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 CC l 4 phase were determined by liquid chromatography with fluorescence detection. Under the optimum conditions, the enrichment factors ( EF s) for metoprolol, bisoprolol, and betaxolol were 180, 190, and 182, and the limits of detection ( LOD s) 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 ( RSD s) 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.