A rapid method for the determination of geniposide,gentiopicroside and baicalin in Longdanxiegan Pill was established.The sample was extracted with 50% methanol,and then purified with C18 solid phase extraction.The extract was separated on an Ultimate XB-C18 (4.6 mm×50 mm,1.8 μm) column at 25 ℃,using acetonitrile-0.1% phosphate acid as mobile phase by gradient elution at flow rate of 0.8 mL?min-1.The effects of experimental conditions,such as different type of column,composition of mobile phase,injection volume,column temperature and flow rate,on separation efficiency of three compounds were investigated,and the equilibrium volume of SPE elution was also discussed.Under the optimal conditions,the method showed good linearity with correlation coefficients not less than 0.999 8.The quantitation limits(LOQs) were in the range of 0.24-0.44 mg/L,and the recoveries ranged from 95% to 99% with RSD no more than 2.8%.The method was rapid and reliable for the quantitation of three compounds in Longdanxiegan Pills.