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

  • Authors: M. Hernández Mesa, C. Cruces Blanco, A.M. García Campaña
  • Reference: Journal of Separation Science 36 (2013) 3050-3058
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 and150 mM SDS as separation buffer. Separation has taken place under a voltage of 25 kV anda temperature of 20 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 2.4g/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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