目的:建立毛细管电泳非接触电导法同时测定牛黄解毒片中大黄酸和大黄素的方法。方法:探讨了缓冲溶液、分离电压和进样条件等因素对分离检测的影响。结果:在电泳介质为15.0 mmol/L Tris-5.0 mmol/L H3BO3(pH=8.0),分离电压20.0 kV的优化条件下,实现了大黄酸和大黄素的同时分离检测,线性范围分别为2.0～50.0μg/mL和4.0～40.0μg/mL,检出限均为2.0μg/mL(S/N=3),加样回收率分别为101～103%和95.0～98.3%。结论:该法可成功测定牛黄解毒片中大黄酸和大黄素含量。 Objective: To establish a method for simultaneous determination of rhein and emodin in bezoar detoxification tablets by capillary electrophoresis non-contact conductivity method. Methods: The effects of buffer solution, separation voltage and injection conditions on the separation and detection were discussed. Results: Simultaneous separation of rhein and emodin was achieved under the optimum conditions of 15.0 mmol / L Tris-5.0 mmol / L H3BO3 (pH = 8.0) and 20.0 kV of separation voltage. The linear range was 2.0 ~ The detection limits were 2.0μg / mL (S / N = 3). The recoveries were 101-103% and 95.0-98.3%, respectively. Conclusion: This method can successfully determine the content of rhein and emodin in Niuhuangjiedu Tablets.