Fe_3O_4@SiO_2-NH_2磁性复合材料对水中全氟化合物的检测研究

Determination of Perfluorinated Compounds in Water Using Fe_3O_4@SiO_2-NH_2 Magnetic Nanoparticles Composites

利用三步法（热溶剂还原法,硅烷化和氨基功能化）制备了Fe3O4@SiO2-NH2磁性纳米复合材料用于水体中全氟化合物的萃取,结合超高效液相色谱-串联三重四极杆质谱（UPLC-MS/MS）技术,建立了水体中7种典型全氟化合物的检测方法。通过扫描电镜（SEM）、透射电镜（TEM）和傅立叶红外光谱（FT-IR）等手段对材料进行表征,详细研究了解析溶剂、解析溶剂体积、解析时间、吸附时间和p H值等因素对萃取效率的影响。结果表明：氨基被成功修饰在Fe3O4@SiO2纳米粒子的表面,Fe3O4@SiO2-NH2磁性纳米材料对目标全氟化合物有较好的萃取效果,在萃取时间为20 min,解析溶剂为3 m L×4含0.28%氨水的甲醇,解析时间为5 min,p H 5.0时,萃取效率最佳。在最优实验条件下,全氟化合物的检出限为0.2~0.5 ng/L,线性范围为1~500 ng/L。方法用于实际水体中目标全氟化合物的检测,样品的加标回收率不低于82.0%。

Fe304@ SiO2 -NH2 magnetic nanoparticles composites were successfully synthesized by three-step method, and used as adsorbents for the extraction and analysis of seven typical perfluori- nated compounds（PFCs） in water solution. In combination with ultra-high performance liquid chro- matography- tandem triple quadrupole mass spectrometry（ UPLC -MS/MS）, a method to determine seven typical perfluorinated compounds in water was established. The synthesized material was char- acterized by TEM, SEM and FT - IR. The influencing factors including desorption solvent, volume of desorption solvent, desorption time, extraction time and pH value of solution were investigated. The result showed that amino was successfully modified on the surface of Fe304 @ SiO2 magnetic nano- particles. Fe30,@ SiO2 -NH2 magnetic nanoparticles composites exhibited a good extraction effect on the target perfluorinated compounds, and the optimum extraction efficiency was achieved as follows： extraction time ： 20 min, desorption solvent ： 3 mL× 4 0.28% ammonia methanol solution, desorp- tion time： 5 min, and pH value： 5. O. Under the optimum conditions, the calibration curves of seven perfluorinated compounds were linear in the range of 1 -500 ng/L, with limits of detection of 0. 2 -0. 5 ng/L. The method was applied in the detection of target perfluorinated compounds in real water with spiked recoveries no less than 82.0%.