Abstract: The content of acetophenone in rubber used for toys was determined by GC-MS. The sample was extracted with acetone by microwave assisted extraction, and purified by passing through silica-gel micro column. An aliquot of the eluant was separated on HP-5MS capillary chromatographic column (30 m×0.25 mm, 0.25 μm), and determined by using electron impact ion source as well as modes of full scan monitoring and selected ion monitoring. Under the selected working conditions for the instrument, the characteristic ions with m/z 77, 51, 120 were selected for quantitative analysis and m/z 105 for quantitative analysis. Linear relationship between values of peak area and mass concentration of acetophenone was kept in the range of 0.1-20 mg·L-1, with lower limit of determination (10S/N)of 1.0 mg·kg-1. Tests for recovery were made by adding acetophenone standard at 3 at concentration levels of 2.00, 4.00 and 10.00 mg·L-1, giving values of recovery in the range of 91.2%-94.5% with values of RSD (n=6) less than 3%.