Objective :To establish HPLC and Thiocyanate methods for the determination of Ester-alkaloids and HgS in Ershiwuweishanhu pills. Methods: Phenomenex Luna C18(2)(4.6 mm×150 mm

5 μm)column was used and the mixture of CH3OH—0.05 mol·L-1KH2PO4—CH3COOH—(CH3)2CHOH (67∶173∶4∶4) was used as the mobile phase: The flow rate was at 1.0 mL·min-1 and the detection wavelength was at 230 nm. The column temperature was at 35 ℃. Results: The calibration curvey of aconitine was Y=6.974×105X-28.1 and the linear range was from 0.096 to 0.480 μg(r=0.999 8).The average recoverys of aconitine was 93.1% with RSD=2.1%. Conclusion: The method is accurate reliable and reproducible. It be used to can control ester-alkaloids and limited HgS in Ershiwuweishanhu pills.