The current routes to couple dispersive liquid-liquid microextraction with capillary electrophoresis are the evaporation of water immiscible extractants and the back-extraction of analytes. In this study, a new methodology for this combination using water-in-oil microemulsion electrokinetic chromatography coupled with normal stacking mode on-line sample concentration was developed to analyze chlorophenols in water samples. The analytes were extracted with tributyl phosphate and the extractant dilution (3×) was directly injected into an electrophoresis buffer (7.7 cm) containing 5% sodium dodecyl sulfate, 78% 1-butanol, 2% 1-heptane, and 15% sodium acetate solution (pH 8.0). This proposed method is very simple and convenient compared to the conventional procedures. The key parameters affecting separation and concentration were systematically optimized. Under the optimized conditions, dispersive liquid-liquid microextraction contributed an enrichment factor of 45-50, and the overall sensitivity improvement was 312-418-fold. Limits of detection between 1.4 and 3.0 ng/mL and limits of quantification between 4.5 and 10.2 ng/mL were achieved. Acceptable repeatability lower than 3.0% for migration time and 9.0% for peak areas were obtained. The developed method was successfully applied for analysis of the chlorophenols in real water samples.
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