纳米Fe_3O_4表面聚合微粒制备及其尿样中二苯甲酮类化合物磁萃取应用

Preparation of nano Fe_3O_4 magnetic polymer microspheres and their application of magnetic solid phase extraction for benzophenones in urine

通过共沉淀法合成出四氧化三铁磁性纳米粒子,再用二氧化硅对磁性纳米粒子表面进行修饰,最后用分散聚合法合成出磁性聚合物微球.利用红外吸收光谱、热重分析和色谱方法对磁性聚合物微球进行结构表征、热稳定性和萃取性能的考察,并将其应用于尿样中二苯甲酮类物质的分离富集,优化了磁萃取条件,建立了尿样中二苯甲酮类物质的高选择性的分离分析方法.实验结果显示,尿样中的2,4-二羟基二苯甲酮、二苯甲酮、2-羟基-4-甲氧基二苯甲酮在0.05300 ng/m L浓度范围内线性关系良好,检测限(S/N=3)为0.05 ng/m L.

Fe_3O_4 nanoparticles were synthesized by chemical co-precipitation of Fe^3＋ and Fe^2＋ under basic condition,and then were coated by SiO_2 by a modified Stober method. The composite was synthesized by dispersion polymerization. The structure and extraction performance of the magnetic polymer microspheres were evaluated by infrared spectrum and HPLC. Then this material was applied to separation and concentration of BPs in urine samples. By optimizing the extraction conditions,high selectivity analytical method for separation of benzophenones in urine had been developed. The experimental results showed that the linear ranges were0. 05—300 ng/m L for benzophenones in urine with the correlation coefficient of above 0. 996 6. The detection limits（ S/N = 3） was 0. 05 ng/m L.