Abstract: A simple, rapid and sensitive method for the determination of deoxyschizandrin and schisandrin B in Schisandra chinensis (Tuecz.) Baill. was established. Bioactive compounds were ultrasonically extracted under the frequency of 40 kHz with 100% methanol for 80 min, and determined by high performance liquid chromatography. The HPLC separation was preformed on a KYA HIQ sil C18 column (250 mm×4.6 mm, 5 μm) at flowrate 1 mL/min and detective wavelength 250 nm, the solvent gradient program was as follow: acetonitrile/water increased linearly from 65% to 85% in the first 30 min, then isocratic for 2 min, acetonitrile/water decreased linearly from 85% to 65% in 2 min; at time 39 min, stopped the program (ready for next injection). Deoxyschizandrin and schisandrin B contents in the root, stem and leaves, and fruits of S. chinensis were determined. The results showed that deoxyschizandrin and schisandrin B were highest in the fruits, then in the stem and leaves, and lowest in the root. Deoxyschizandrin content in stem and leaves was equal to fruits, which may suggest that stem and leaves has the value to be explored as the medicinal substitute of fruits of S. chinensis.