固相微萃取-高效液相色谱法测定水中的酞酸二(2-乙基己基)酯

Determination of Trace DEHP in Aqueous Solution by Solid Phase Microextraction Coupled with High Performance Liquid Chromatography

分别采用PDMS、PDMS/DVB、CWX/DVB三种萃取头,应用固相微萃取与高效液相色谱联用技术(SPME HPLC)分析了水溶液中的痕量酞酸二(2 乙基已基)酯(DEHP)。实验发现,PDMS/DVB萃取头的萃取效果较其他两种萃取头理想;对SPME的萃取条件进行了优化,建立了水中痕量DEHP的SPME HPLC分析方法,并对实际水样进行了分析。该方法的线性范围为0.62～15.60mg/L,相关系数为0.9991,检出限为0.06mg/L(3σ,n=11),相对标准偏差(RSD)为3.3%,回收率为89.9%～101.3%。

A rapid determination method for trace DEHP in aqueous solution by solid phase microextraction (SPME) coupled with high performance liquid chromatography (HPLC) was developed. In this experiment, the extraction effects of three solid phase microextraction fibers (PDMS,PDMS/DVB and CWX/DVB)were compared. It was found that PDMS/DVB had the best effect on the determination for trace DEHP. The variables affecting in SPME-HPLC were optimized, such as extraction time, desorption time and pH. The linear range was from 0.62 to 15.60 mg/L with the correlative coefficient of 0.999 1. The method was used for the determination of trace DEHP in leachate of Qingshan landfill and leachate of Liufang landfill and distilled water in plastic tub. The recoveries were from 89.9% to 101.3%. This method is fast, convenient, sensitive, solvent-free, and suitable for the determination of trace DEPH in aqueous solution.