玩具用橡胶中苯乙酮用丙酮作溶剂微波辅助萃取,经硅胶小柱净化后,用气相色谱-质谱法测定其含量。采用HP-5MS毛细管色谱柱(30 m×0.25 mm,0.25 μm)进行分离,电子轰击离子源及全扫描和选择离子监测模式进行测定。在选择的仪器工作条件下,选择苯乙酮的定性离子为m/z 77,51,120,选择定量离子为m/z 105。苯乙酮的质量浓度在0.1~20 mg·L-1浓度范围内与峰面积呈线性关系,测定下限(10S/N)为1.0 mg·kg-1。在2.00,4.00,10.00 mg·L-1标准苯乙酮的3个浓度水平上,苯乙酮的回收率在91.2%~94.5%之间,相对标准偏差(n=6)小于3%。

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%.