磁固相萃取/气相色谱-质谱法分析水样中的16种邻苯二甲酸酯类化合物

Determination of 16 Phthalate Acid Esters in Water Samples by Magnetic Solid Phase Extraction/Gas Chromatography-Mass Spectrometry

合成了一种由Fe3O4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1 min,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0.035～0.255μg/L和0.115～0.845μg/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。

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 chromatography-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 amount of elution solvent,desorption time,adsorption time and pH value of water sample,were investigated.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 detection limits（S/N=3） for 16 PAEs were in the range of 0.035-0.255 μg/L and the quantitation limits（S/N=10） were 0.115-0.845 μg/L.The developed method was successfully applied in the analysis 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.