建立了固相微萃取-气相色谱-串联质谱法测定水生蔬菜中35种多氯联苯的方法。采用100 μm聚二甲基硅氧烷萃取纤维，在萃取温度60 ℃、转动速度250 r/min的条件下萃取30 min，经气相色谱进样口280 ℃解吸6 min后，采用气相色谱-串联质谱法在时间选择反应监测模式下进行测定，外标法定量。结果表明，35种目标物在10～500 μg/L内呈良好线性，线性相关系数均大于0.999，方法检出限为0.55～17.22 ng/kg；在0.01 mg/kg加标水平的平均回收率为72.3%～117.3%，相对标准偏差为1.2%～11.2%。该方法简便、快速、灵敏、准确，适用于水生蔬菜中多种多氯联苯残留量的快速测定。

A solid-phase microextraction coupled with gas chromatography-tandem mass spectrometry method was developed for the determination of 35 polychlorinated biphenyls in aquatic vegetables.Samples were extracted with 100 μm polydimethylsiloxane at 60 ℃ for 30 min, and stirring at 250 r/min.After desorbed 6 min at 280 ℃ in gas chromatograph, sample extracts were injected and analyzed by GC-MS/MS at time selective reaction monitoring mode, and quantified by external standard method.The results showed that 35 target analysts displayed good linear relationships over concentration range of 10-500 μg/L, and correlation coefficients above 0.999.The limits of detection were 0.55-17.22 ng/kg.The average recoveries of 35 compounds at two spiked levels of 0.01 mg/kg ranged from 72.3% to 117.3%, with relative standard deviations of 1.2% to 11.2%.The advantages of simplicity, rapidness, sensitiveness and accuracy of the method was suitable for rapid detection of PCBs residues in aquatic vegetables.