二氧化硅/聚苯乙烯复合微球的制备及作为固相萃取填料的研究

Preparation of SiO_2/PS composite microsphere and its application as solid-phase extraction sorbent

以分散聚合法制备了二氧化硅/聚苯乙烯单分散复合微球,以红外光谱、透射电镜(TEM)、扫描电镜(SEM)等手段对其进行了表征。以合成的二氧化硅/聚苯乙烯作为固相萃取填料制作固相萃取小柱。通过固相萃取与液相色谱联用,测定了水中邻硝基酚、间硝基酚、对硝基酚和辛基酚、壬基酚,考察了固相萃取条件对固相萃取柱性能的影响,选择了最佳的色谱分离条件。结果表明,自制固相萃取小柱对水中硝基酚、烷基酚的萃取率高,与HPLC联用测定结果重现性好,邻硝基酚、间硝基酚、对硝基酚、辛基酚、壬基酚的最低检出限分别为0.90、0.72、0.62、0.38和0.41μg/L。

The silicon dioxide（SiO2）/ polystyrene（PS） composite microspheres were prepared by dispersion polymerization.The compositions,structures,surface morphologies and particle sizes of the microspheres were characterized by FT-IR,SEM and TEM.Using SiO2/ PS composite microspheres as solid-phase extraction（SPE） sorbents for selective extraction of o-nitrophenol,m-nitrophenol,nitrophenol and octylphenol,nonylphenol in water,methanol was used as an eluent,and the eluent was concentrated to 1 mL under gentle nitrogen gas flow.The nitrophenols and the alkylphenols were determined by high performance liquid chromatography.The effects of the conditions on the extraction performance of SPE column were investigated.The analytical conditions of HPLC were optimized.The results show that the SPE sorbent had high extraction efficiency to nitrophenol and alkylphenol in water.The method had good reproducibility.The detection limits for o-nitrophenol,m-nitrophenol,p-nitrophenol,octylphenol and nonylphenol were 0.90,0.72,0.62,0.38 and 0.41μg/L,respectively