Abstract: The micellar electrokinetic capillary chromatography(MECC) method is applied to the separation and determination of syringin(SR), herniarin(7-MC), daphnin(DN), daphnetin(DP) and umbellifrone(7-HC) in Cortex Daphnes. The background electrolyte system, composed of 20 mmol/L borax-boric acid buffer(pH 9.0)-10 mmol/L SDS was found to be the most suitable solution for this separation. The five analytes were completely separated in 8 min using an applied voltage of 20 kV. The linear calibration ranges were 1.0~100 μg/mL for SR, 1.5~100μ g/mL for 7-MC, 5.0~75 μg/mL for DN, 5.0~75 μg/mL for DP, 1.0~75μg/mL for 7-HC, and the detection limits of the five analytes were 0.3, 0.5, 1.7, 1.7 and 0.3 μg/mL, respectively. The method shows good selectivity, repeatability, linearity and sensitivity, and several different samples were successfully analyzed.