磁固相萃取/气相色谱一质谱法分析水样中的16种邻苯二甲酸酯类化合物

摘要

A nanocomposite comprised of Fe3O4 magnetic nanoparticles ( MNPs) and multi-walled carbon nanotubes( MWCNTs) was synthesized, and used as adsorbent in the determination of 16 PAEs in water samples by magnetic solid phase extraction ( MSPE) and quantification by gas chroma tography - mass spectrometry(GC - MS). The synthesis nano material was characterized by Fourier transform infrared spectroscopy. The factors affecting the extraction efficiency, such as type and a mount of elution solvent, desorption time, adsorption time and pH value of water sample, were in vestigated. The optimized conditions were as follows: elution solvent: 1 mL toluene - acetone (1 ∶ 4); desorption time; 1 min; adsorption time; 3 min; pH of water sample: 5.0-7.0. The detec tion limits(S//V =3) for 16 PAEs we're in the range of 0. 035 -0. 255 u,g/L and the quantitation lim its (S/N = 10) were 0. 115 -0. 845 μg/L. The developed method was successfully applied in the a-nalysis of 16 PAEs in tap water, lake water and river water. The recoveries at 3 spiked levels ranged from 87% to 112% with RSDs of 1. 3% - 11. 9% . The results demonstrated that the MSPE method could be rapidly and effectively used in the monitoring of trace PAEs contaminants in water sample.%合成了一种由Fe3 O4磁性纳米粒子(MNPs)和多壁碳纳米管(MWCNTs)组成的复合纳米材料,用于水样中16种邻苯二甲酸酯类化合物(PAEs)的磁固相萃取(MSPE),并结合气相色谱-质谱(GC - MS)法进行定量分析.合成的纳米材料用傅立叶变换红外光谱表征.为提高萃取效率,优化了解析溶剂的种类和用量、解析时间、萃取时间、水样pH值等影响因素,确定最佳萃取条件为:解析溶剂为1 mL甲苯-丙酮(1:4),解吸时间 1min,萃取时间3 min,水样pH 5.0～7.0,方法的检出限(S/N=3)和定量下限(S/N=10)分别为0.035 ～0.255 μg/L和0.115 ～0.845 μg/L.将该方法用于自来水、湖水和河水样品的分析,加标回收率为87％～112％,相对标准偏差为1.3％～11.9％.MSPE方法可用于水样中痕量PAEs污染物的快速、有效监测.