固相萃取－气相色谱法同时测定水中的酞酸酯类环境激素

Determination of 4 kinds of phthalate esters simultaneously in water by solid phase extraction combined with gas chromatography detector

为了解我国市售饮用水中酞酸酯类环境激素的污染状况,采用固相萃取技术作为水样的前处理手段,结合气相色谱对5种品牌塑料灌装饮用水、18L桶装水及某市自来水中4种酞酸酯[邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异丁基酯(DiBP)、邻苯二甲酸二丁基酯(DBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)]进行分析测定。并使用C18固相萃取柱,研究了水中酞酸酯类环境激素的固相萃取预富集方法,考虑影响回收率的3个主要因素,即洗脱溶剂、水样流速、洗脱溶剂用量。最后确定最佳萃取条件为:洗脱溶剂乙酸乙酯,水样流速4mL.min-1,洗脱体积3mL。实验结果表明,在所有测定的水样中,除DEP外,其余三种均被检测到,其中DiBP含量在0.017～0.057μg.mL-1之间,DBP为0.019～0.222μg.mL-1,DEHP为0.009～0.061μg.mL-1。

In order to assess the contaminant status of phthalate esters in drinking water, a solid phase extraction method combined with gas chromatography was developed and validated for the determination of four phthalate esters（ diethylphthalate（ DEP ）, di- iso- butyl phthalate （ DiBP）, dibutyl phthalate （ DBP）, di- （ 2 - ethylhexyl） phthalate （DEHP）） simultaneously in five brand drinking water, 18L barreling water and tap water samples. Moreover the method of preconcentration of phthalate ester in water was systematically studied. Several factors which may affect recoveries of analyses were optimized. These include type of eluting solvent, flow rate of water and amount of eluting solvent. The optimized conditions were as follows： eluting solvent was ethyl acetate, flow rate of water was 4mL · min^-1 , volume of eluting was 3mL. The results indicated that DiBP, DBP and DEHP were the main contaminants in all water samples, the content of DiBP was between 0.017 and 0.057μg · mL^-1, DBP was 0.019-0.222μg · mL^-1, DEHP was0.009-0.061μg · mL^-1.