Li Ying, Wang Tianran, Hashi Yuki, Li Haifang, Lin Jin-Ming
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, China.
Talanta. 2009 Jun 15;78(4-5):1429-35. doi: 10.1016/j.talanta.2009.02.046. Epub 2009 Mar 5.
Determination of brominated flame retardants in electrical and electronic equipments (EEE) was achieved through microwave-assisted extraction (MAE) and gas chromatography-mass spectrometry. Polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) including mono-brominated through deca-brominated congeners were qualified and quantified with good linearity (0.9963-0.9998) and repeatability (RSD, 1.1-8.1%). Multivariable orthogonal experimental design was used to optimize the MAE parameters. Extraction temperature and time were the most significant factors for extraction process. The extractants were cleaned up with SPE method after extraction. Recoveries of spiked blank samples ranged from 72.4% to 108.4% for most of the analytes. The method was applied to the determination of PBBs and PBDEs in several kinds of real EEE samples. It was found that no detectable level of PBBs was detected among them. Different contents of PBDEs were tested in the tested samples and the total contents ranged from 25.0 ng g(-1) to 194.0 ng g(-1). The proposed approach demonstrated an environmentally friendly and convenient alternative, which only consumed 10mL hexane to microwave extraction for 10min at 100 degrees C.
通过微波辅助萃取(MAE)和气相色谱-质谱联用技术实现了对电气和电子设备(EEE)中溴化阻燃剂的测定。对包括一溴代至十溴代同系物在内的多溴联苯(PBBs)和多溴二苯醚(PBDEs)进行了定性和定量分析,线性良好(0.9963 - 0.9998),重复性好(相对标准偏差,1.1 - 8.1%)。采用多变量正交实验设计优化微波辅助萃取参数。萃取温度和时间是萃取过程中最重要的因素。萃取后用固相萃取(SPE)方法对萃取剂进行净化。加标空白样品中大多数分析物的回收率在72.4%至108.4%之间。该方法应用于几种实际电气和电子设备样品中多溴联苯和多溴二苯醚的测定。结果发现其中未检测到可检测水平的多溴联苯。在所测试的样品中检测到了不同含量的多溴二苯醚,总含量在25.0 ng g⁻¹至194.0 ng g⁻¹之间。所提出的方法是一种环保且便捷的替代方法,在100℃下微波萃取10分钟仅消耗10mL己烷。