固相萃取高效液相色谱法测定水中邻苯二甲酸酯类环境激素

Analysis of Phthalic Acid Esters of Environmental Hormone in Water Using Solid Phase Extraction and High Performance Liquid Chromatography

建立了以HLB固相萃取柱和反相液相色谱法测定水中8种邻苯二甲酸酯类环境激素的方法,利用正交试验进行萃取条件的优化,确定固相萃取的优化条件为:洗脱剂组成为V(甲醇)∶V(乙醚)=1∶19,洗脱速率为1 0mL min,洗脱体积为9mL,清洗剂组成为V(甲醇)∶V(水)=1∶19。8种物质峰面积对浓度进行线性回归的相关系数均大于0 999,最低检出限为0 10～0 62μg L,回收率为75 1%～115 5%,相对标准偏差为0 9%～2 2%。同时将该方法应用于废水中邻苯二甲酸酯类环境激素的测定,检出DEP,BBP,DBP和DEHP4种邻苯二甲酸酯类环境激素。

A method for the determination of eight phthalic acid esters of environmental hormone in water samples by using solid-phase extraction on HLB cartridge and reversed-phase liquid chromatography was established. Several factors that would affect recoveries of analytes were optimized by orthogonal design. The optimized results were as follows: eluting solvent was V(methanol)∶V(ethyl ether)=1∶19, eluting rate 1.0 mL/min, elution volume 9 mL, and washing solvent was V(methanol)∶V(H_2O)=1∶19. Linear correlation coefficient (r) was over 0.999. The limits of detection were between 0.10 and 0.62 μg/L. The recoveries of eight phthalic acid esters were between 75.1% and 115.5%. The repeatability expressed as relative standard deviation was between 0.9% and 2.2%. The method was applied to analyze phthalic acid esters of environmental hormone in wastewater. Four kinds of phthalic acid esters (DEP, BBP, DBP and DEHP) were checked out.