塑料电子电气产品中四溴双酚A的微波辅助萃取-衍生气相色谱-质谱法测定

Determination of Tetrabromobisphenol A in Plastic Electrical and Electronic Products by Microwave-Assisted Extraction-Derivatization with Gas Chromatography-Mass Spectrometry

利用甲苯/甲醇(10:1,体积比)溶液微波辅助萃取塑料电子电气样品,用正己烷沉淀萃取液中的高聚物,以N,O-双(三甲基硅烷基)三氟乙酰胺为衍生化试剂,对萃取液进行衍生化反应,采用气相色谱-质谱总离子流和选择离子流对四溴双酚A进行定性定量测定。对衍生化时间、衍生化温度、衍生化试剂用量、沉淀试剂用量等前处理条件进行了优化,并进行了线性关系、回收率、精密度等试验。结果表明:本方法线性范围0.05～50mg/L,相关系数为0.9992,检测低限为2mg/kg,回收率在91.0%～97.9%之间,相对标准偏差小于7%。

The plastic electrical and electronic sample was extracted by toluene/methanol （10：1, volume ratio） solution, and the polymer in the extraction solution was precipitated by n-hexane. After purification, the extraction solution was derivated by taking N,O-bis（trimethylsilyl） trifluoroacetamide as derivatization agent. The qualitative and quantitative analysis for tetrabromobisphenol A was carried out by total ion chromatogram and selected ion chromatogram with gas chromatography-mass spectrometry. The pretreatment conditions, such as derivatization time and temperature, use amount of derivatization agent and precipitation agent, were optimized. The tests of linear correlation, recovery rate and precision were performed. The results show that： the linearity range of the testing method is 0.05-50mg/L, the correlation coefficient is 0.9992, the lowest detection limit is 2mg/kg, the recovery rate and relative standard deviation are 91.0%-97.9% and less than 7% respectively.