Objective: To establish a determination method for senegenin and polygalacic acid in Naolibao pills by capillary electrophoresis. Method: The separation was carried out in an uncoated fused silica capillary (75 μm×50 cm). The running voltage was 25 kV. The buffer was 20 mmol ·L-1 Na2B4O7 containing 20% methanol. The wavelength was at 210 nm. Result: senegenin was linear in the range of 13.25-212 mg ·L-1(r=0.997 1) and polygalacic acid was linear in the range of 12.5-200 mg ·L-1 (r=0.997 7). The average recoveries of senegenin and polygalacic acid in Naolibao pills were 100.5% and 100.6% respectively. Conclusion: This method is proved to be simple, rapid and accurate, and can be used as a new method for the quality control of Nailibao pills.