OBJECTIVE： To establish a method for the simultaneous determination of gallic acid， protocatechuic acid and hyperin in Euphorbia helioscopia from Guizhou， and to lay a foundation for the formulation of quality standard of E. helioscopia and its related products. METHODS： HPLC method was adopted. The determination was performed on X-brige C18 column with mobile phase consisted of acetonitrile-1％glacial acetic acid （gradient elution） at a flow rate of 1 mL/min. The detection wavelengths were set at 271 nm， 259 nm and 256 nm for gallic acid， protocatechuic acid and hyperoside， respectively. The column temperature was 30 ℃， and sample size was 10 μL. RESULTS： The linear range of gallic acid， protocatechuic acid and hyperoside were 0.005 6-0.089 6 （R2＝0.999 9）， 0.003 6-0.057 3 （R2＝0.999 7） and 0.017 2-0.275 5 mg/mL （R2＝1.000 0）， respectively. The detection limits were 31.43， 39.64， 49.05 ng/mL， respectively. The quantitation limits were 78.58， 99.10， 122.63 ng/mL， respectively. RSDs of precision （n＝6）， stability （n＝6） and reproducibility （n＝9） tests were all lower than 3.0％. The sample recovery rates were 100.24％-101.64％ （RSDs＜2.0％， n＝9）.  CONCLUSIONS： The developed HPLC method is simple， accurate and suitable for the simultaneous determination of gallic acid， protocatechuic acid and hyperin in E. helioscopia from Guizhou.