OBJECTIVE To develop a method for the determination of zaleplon in its pharmaceutical material and preparation METHODS A RP-HPLC method was used with Waters Spherisorb S5 ODS2 (5μm, 4.6 mm×250 mm) column. The mobile phase was a mixture of methanol -0.01 mol·L^-1 phosphoric acid (57∶43) and the flow rate was 1.0 mL·min^-1, and column temperature 25℃, with the detection wavelength at 231 nm RESULTS The precision and stability were fine. The linear correlation was observed from the concentrations of 0.011 3 mg·mL^-1 to 0.067 5 mg·mL^-1 (r=0.999 8). The average recovery was 99.7%. Resolution between zaleplon peak and other peaks met the requirements CONCLUSION The method was convenient, selective and reproducible.