A novel method of microchip capillary electrophoresis with electrochemiluminescence (ECL) detection for the rapid determination of procaine hydrochloride was developed.Tris (2,2’-bipyridyl)-ruthenium (Ⅱ)(Ru(bpy)2+3) was chosen as ECL reagent,a 300 μm diameter platinum disc working electrode was embedded in a titanium tube which provides an adequate holding for the working electrode and acts as counter electrode，and an Ag/AgCl wire reference electrode was inserted in the ECL detection cell to form a three-electrode system.The factors influencing the performances of separation and detection,such as pH values of running buffer and detection buffer,detection potential and separation voltage,were investigated.Under the following optimized conditions:running buffer:10 mmol/L phosphate buffer (pH 4.0),separation voltage:300 V/cm,detection solution:5 mmol/L Ru(bpy)2+3 in 50 mmol/L phosphate buffer(pH 7.0),detection potential:1.25 V,procaine hydrochloride was separated and detected in 40 s.The linear response of procaine hydrochloride ranged from 10 μg/mL to 2 000 μg/mL(r2=0.999 1).The limits of detection(S/N=3) was 3.0 μg/mL.The spiked recoveries were in the range of 97%-99% with relative standard deviations of 1.8%-2.2%.This method was simple,rapid and reliable,and could be used for the determination of procaine hydrochloride content in injection.