AIM: To develop a HPLC method to determine emodin and chrysophanol in Shierwei Chiyinkang Powder (Gypsumseu Calcitum, Radix et Rhizoma Rhei, Herba Asari, Rhizoma Chuanxiong, Rhizoma et Radix Notopterygii, Radix Gentianae, Pericarpium Zanthoxyli, etc.). METHODS: The sample was made referring to China Pharmacopoeia(2000) and determined by HPLC. The separation was performed on a Shim pack CIC ODS column (150mm?5mm, 4.5?m) with a mobile phase of methanol 0.1% H 3PO 4 solution (40∶9). The flow rate was 1.3mL?min -1 and the detective wavelength was set at 254nm. RESULTS: The emodin and chrysophanol in sample were separated. The square linear ranges were 0.52～5.28?m?mL -1 ( r =0.9999) and 0.96～9.60?m?mL -1 ( r=0.9999 ), respectively, and the average recoveries were 98.62% and 98.57% for emodin and chrysophanol, respectively. CONCLUSION: This method is sensitive and accurate for the determination of emodin and chrysophanol in the sample.