Abstract: Ten kinds of wood preservatives of chlorophenols and pyrethroids in wooden children's products were determined simultaneously using solid phase extraction coupled with gas chromatography-tandem mass spectrometry (SPE-GC-MS/MS). The sample was ultrasonically extracted with methanol. The extract was evaporated and then derivatised with acetic anhydride. Finally the solution was purified using Oasis HLB SPE column. The separations were performed on an Agilent HP-5MS column (30 m×0.25 mm×0.25 μm)， then were determined by MS/MS and quantified by internal standard method. Procedures for extraction and purification were carefully optimized. The method was proved to be linear over a wide range of concentrations for all analytes with the correlation coefficients greater than 0.999 3. Limits of detection (LODs) and limits of quantification (LOQs) are in the range of 0.001—0.05 mg/kg and 0.002 5—0.2 mg/kg, respectively. Average recoveries of target compounds (spiked at three concentration levels) are in the range of 85.2%—100.1%. Intraday and interday repeatability (RSD, n=6) of the proposed method are vary of 0.6%—9.1% and 2.3%—7.2%， respectively. The proposed method was used to monitor preservatives in commercial wooden toys, and some preservatives were found.