The method of reversed-phase high performance liquid chromatography was established for the determination of effective components in OC-CS spray using double wavelength UV detection. The method was utilized under following con-ditions: a column of Kromasil C18 (250 mm×4.6 mm, 5 μm), mobile phase consisting of methanol/water (80/20) at a flow rate of 0. 8 mL/min, column temperature of 25 ℃, and the UV detection at 227 nm and 300 nm. Three key compo-nents in OC-CS spray could be distinguished clearly, including o-chlorobenzalmalononitrile (CS), oleoresin capsicum (OC) and dihydrocapsaicin (DC). This method has the advantages of fast, simple and satisfactory linear relationship be-tween UV absorption and concentration. It may be considered to turn into a standard method for detection of related compo-nents in the spray.