We have employed a high-sensitivity off-line coupled with on-line preconcentration method, cloud-point extraction (CPE)/cation-selective exhaustive injection (CSEI) and sweeping-MEKC, for the analysis of malachite green. The variables that affect CPE were investigated. The optimal conditions were 250 g/L of Triton X-100, 10% of Na(2)SO(4) (w/v), heat-assisted at 60 degrees C for 20 min. We monitored the effects of several of the CSEI-sweeping-MEKC parameters - including the type of BGE, the concentrations of SDS, the injection length of the high-conductivity buffer, and the injection time of the sample - to optimize the separation process. The optimal BGE was 50 mM citric acid (pH 2.2) containing 100 mM SDS. In addition, electrokinetic injection of the sample at 15 kV for 800 s provided both high separation efficiency and enhanced sweeping sensitivity. The sensitivity enhancement for malachite green was 1.9 x 10(4) relative to CZE; the coefficients of determination exceeded 0.9928. The LOD, based on an S/N of 3:1, of CSEI-sweeping-MEKC was 0.87 ng/mL; in contrast, when using off-line CPE/CSEI-sweeping-MEKC the sensitivity increased to 69.6 pg/mL. This proposed method was successfully applied to determine trace amounts of malachite green in fish water samples.