Abstract: OBJECTIVE To establish an SPE-HPLC method for the determination of six alkaloids in Fengshigutong tablet. METHODS Welch XB-C₁₈ column(4.6 mm×250 mm, 5 μm) was used, the mobile phase was a mixture of acetonitriletetrahydrofuran (25:15) (A)-0.05%ammonium acetate at a flow rate of 1.0 mL·min^-1 for gradient elution, the column temperature was 30℃ with analysis was monitored at 235 nm, injection volume 10 μL. RESULTS The good linearity with peak areas was achieved in the rang of 162.4-8 121 ng(r=1.000 0), 24.96-1 248 ng(r=1.000 0), 58.03-2 902 ng(r=1.000 0), 17.26-863.0 ng(r=1.000 0), 20.16-1 008 ng(r=1.0000) and 19.90-995.0 ng(r=1.000 0) for benzoyl new aconitine, benzoyl aconitine, benzoyl methacholine, new aconitine, hypaconitine and aconitine, the average recoveries in the range of 88%-98%, RSD was 1.8%-2.4%. CONCLUSION The method is accurate and reliable, and it is suitable for the analysis of alkaloids content in Fengshigutong tablets.