Abstract: A simple and effective method has been developed for the rapid determination of ortho-phenylphenol (OPP) in wooden toys using GC-MS technique. The sample was firstly extracted with methanol by ultrasonication, followed by an acetylating with acetic anhydride, and finally analyzed using GC-MS. It was found that the linearity of OPP by this method was ranged from 0.1 mg/L to 4.0 mg/L, its detection limit was as low as 0.01 mg/L. The recoveries were ranged from 85%~101% with RSD of 3.29% and 3.52%. The results indicated that the method is not only suitable for detecting OPP in wooden toys, but also has the potential application in analysis of OPP in other materials.