表面分子印迹磁性固相萃取-液相色谱-荧光光谱法测定河水中双酚A

Preparation and evaluation of superparamagnetic surface molecularly imprinted polymer submicron-particles for selective extraction of bisphenol a in river water

通过原子转移自由基聚合(Atom Transfer Radical Polymerization-ATRP)法制备核壳结构单分散性磁性亚微米粒子(Fe3O4@MIPs),并建立了磁性固相萃取-高效液相色谱荧光光谱(MSPE-HPLC–FLD)测定河水中环境类雌激素双酚A(BPA)的方法。利用透射电镜和傅立叶红外光谱仪对Fe3O4@MIPs进行了表征,研究了溶液pH、磁性亚微米粒子用量、洗脱溶剂和体积等因素对分析的影响。结果表明,在以Waters C18柱为分析柱,流动相为甲醇溶液,激发波长275nm和发射波长305nm为条件时,测定双酚A在0.1～20 ng/mL范围内线性关系良好(r2>0.9993)。回收率为95.6%～108.4%,方法检出限为0.05 ng/mL。该方法能用于环境中痕量双酚A的快速测定。

Molecularly imprinted polymer （MIP） coated Fe304 submicron-particles （Fe3O4 @ MIP ） were synthesized by atom transfer radical polymerization （ATRP） and used as magnetic solid-phase extraction （MSPE） highly special sorbents for trace bisphenol A （BPA） from river water. The morphological and polymeric characteristics of the Fe3O4@ MIP were characterized by transmission electron microscopy and Fourier transform infrared spectroscopy. Various parameters such as the pH of sample, the amount of Fe3O4 @ MIP sorbents, the extraction time, and the desorption conditions were optimized. After separation by Waters C18 column, the sample is detected at the excitation and emission fluorescence at wavelengths of 275 nm and 305 nm. Good linearity （r^2 〉 0. 9993） for all calibration curves was obtained, and the limit of detection （LOD） for BPA was 0. 05 ng/mL in Xiangjiang river samples. The recoveries of spiked BPA in the samples were 95.6% - 108. 4%. The method was sensitive and simple, and was suitable for the rapid determination of BPA in real environment samples.