A new method for the determination of arecoline in Semen Arecae decoction pieces by microchip capillary electrophoresis with contactless conductivity detection (MCE-CCD) was proposed. The effects of various electrophoretic operating parameters on the analysis of arecoline were studied. Under the optimal conditions, arecoline was rapidly separated and detected in 1 rain with good linearity over the concentration range of 20 1500 uM (r2=0.9991) and the detection limit of 5 uM (S/N=3). The method was used for the analysis of arecoline satisfactorily with a recovery of 96.8 -104%.