4.5 Article

Green methodology based on dispersive liquid-liquid microextraction and micellar electrokinetic chromatography for 5-nitroimidazole analysis in water samples

Journal

JOURNAL OF SEPARATION SCIENCE
Volume 36, Issue 18, Pages 3050-3058

Publisher

WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201300535

Keywords

CE; Dispersive liquid-liquid microextraction; 5-Nitroimidazoles; Water samples

Funding

  1. Junta de Andalucia [P08-AGR-4268]
  2. Plan Propio of the University of Granada

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Dispersive liquid-liquid microextraction has been proposed as an extraction technique combined with micellar electrokinetic chromatography (MEKC) for the analysis of eight 5-nitroimidazole compounds, including some metabolites, in water samples. Determination has been carried out using a diode array detector, employing 20 mM sodium phosphate and 150 mM SDS as separation buffer. Separation has taken place under a voltage of 25 kV and a temperature of 20 degrees C. Samples were prepared in a buffer without micelles and they were hydrodynamically injected at 50 mbar for 25 s, producing a sweeping effect on the analytes for increasing sensitivity. Different factors involved in the dispersive liquid-liquid microextraction procedure were optimized, such as sample pH, nature, and volume of extraction and dispersive solvents in the mixture, percentage of NaCl added to sample and shaking time after the injection of the extraction and dispersive solvents. The method was characterized for water samples, achieving detection limits lower than 2.4 mu g/L. Trueness was checked in river, tap, and bottled water. Dispersive liquid-liquid microextraction combined with MEKC constitutes an easy, cheap, and green alternative for 5-nitroimidazole analysis in environmental water samples.

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