基于苯基功能化纤维状Fe3O4@SiO2@KCC-1的磁性固相萃取-高效液相色谱测定环境水样中的邻苯二甲酸酯

Magnetic Solid-Phase Extraction of Phthalate Esters from Environmental Water Samples using Fibrous Phenyl-functionalized Fe3O4@SiO2@KCC-1

本文采用共聚法制备了一种新型苯基功能化纤维状Fe3O4@SiO2@KCC-1(Fe3O4@SiO2@KCC-1-phenyl)材料,用于环境水样中邻苯二甲酸酯的磁性萃取.制备的Fe3O4@SiO2@KCC-1-phenyl展现了单分散的球形纤维状、较强的磁性(29 emu/g)和一个丰富的π电子体系.研究和优化了洗脱溶剂的种类、吸附剂的用量、萃取时间和可重复使用性等因素对分析物萃取效率的影响.在最佳条件下,用高效液相色谱方法,采用Fe3O4@SiO2@KCC-1-phenyl萃取分离及测定环境水样中的邻苯二甲酸酯类化合物.结果表明,本方法具有良好的线性(0.1~20 ng/mL)、低的检测限(7.5~29μg/L,S/N=3).将该方法应用于不同环境水样中邻苯二甲酸酯类化合物的测定,回收率为93%~103.4%,相对标准偏差为0.8%~8.3%.

A new kind of phenyl-functionalized magnetic fibrous mesoporous silica(Fe3 O4@Si O2@KCC-1-phenyl) was prepared by copolymerization as an efficient adsorbent for the magnetic extraction of phthalate esters from environmental water samples. The obtained Fe3 O4@Si O2@KCC-1-phenyl showed monodisperse fibrous spherical morphology, fairly strong magnetic response(29 emu/g), and an abundant π-electron system, which allowed rapid isolation of the Fe3 O4@Si O2@KCC-1-phenyl from solutions upon applying an appropriate magnetic field. Several variables that affect the extraction efficiency of the analytes,including the type of the elution solvent, amount of adsorbent, extraction time and reusability, were investigated and optimized. Under optimum conditions, the Fe3 O4@Si O2@KCC-1-phenyl was used for the extraction of four phthalate esters from environmental water samples followed by high-performance liquid chromatographic analysis. Validation experiments indicated that the developed method presented good linearity(0.1-20 ng/m L), low limit of detection(7.5-29 μg/L, S/N =3). The proposed method was applied to the determination of phthalate esters in different real water samples, with relative recoveries of 93%-103.4%and relative standard deviation of 0.8%-8.3%.