An HPLC method for determination of naringin, hesperidin and neohesperidin in Muxiang Fenqi Pill was developed.The anal. was carried out with an Agilent C18 (4.6 mm×250 mm, 5 μm) column and the mobile phase of acetonitrile-1% phosphoric acid (21:79).The flow rate was 1.0 mL·min-1, and column temperature was 30°C.The detection wavelength was set at 283 nm.The calibration curve was linear within the range of 0.1108-1.2188 μg (r=0.9994, n=6), 0.2268-2.4948 μg (r=0.9997, n=6) and 0.0848-0.9328 μg (r=0.9994, n=6) for narigin, hesperidin and neohesperidin.The average recoveries were 97.5% (RSD 0.80%, n=6), 99.0% (RSD 1.7%, n=6) and 98.2% (RSD 1.6%, n=6) resp.The results showed this method was reproducible, sensitive and accurate for determination of naringin, hesperidin and neohesperidin in Muxiang Fenqi Pill.