A sensitive,simple and low-cost method based on capillary electrophoresis(CE) with electrochemical(EC) detection at a carbon fiber microdisk electrode(CFE) was developed for the determination of nicotine.Effects of detection potential,concentration and pH value of the phosphate buffer,and injection time as well as separation voltage were investigated.Under the optimized conditions:a detection potential of 1.20 V,40 mmol/L phosphate buffer(pH 2.0),a sample injection time of 10 s at 10 kV and a separation voltage of 16 kV,the linear range obtained was from 5.0×10-7 mol/L to 1.0×10-4 mol/L with a correlation coefficient of 0.9989 and the limit of detection(LOD,S/N=3) obtained was 5.0×10-8 mol/L.The method was also used to determine the nicotine in cigarettes.Nicotine amount ranged from 0.211 mg/g to 0.583 mg/g in the pipe tobacco of seven brands of cigarette and the amount in one cigarette varied from 0.136 mg/cigarette to 0.428 mg/cigarette. A sensitive, simple and low-cost method based on capillary electrophoresis (CE) with electrochemical (EC) detection at a carbon fiber microdisk electrode (CFE) was developed for the determination of nicotine. Effects of detection potential, concentration and pH value of the phosphate buffer, and injection time as well as separation voltage were investigated. Under the optimized conditions: a detection potential of 1.20 V, 40 mmol / L phosphate buffer (pH 2.0), a sample injection time of 10 s at 10 kV and a separation voltage of 16 kV, the linear range obtained was from 5.0 × 10 -7 mol / L to 1.0 × 10 -4 mol / L with a correlation coefficient of 0.9989 and the limit of detection (LOD, S / N = 3) was was 5.0 × 10 -8 mol / L. The method was also used to determine the nicotine in cigarettes. The Nicotine amount ranged from 0.211 mg / g to 0.583 mg / g in the pipe tobacco of seven brands of cigarette and the amount in one cigarette varied from 0.136 mg / cigarette to 0.428 mg / cigarette.