固相萃取-反相高效液相色谱法测定水中的邻苯二甲酸酯  

Determination of phthalate esters in water by SPE-RPHPLC

作　　者：马继平[1] 李茉[1] 赵秀华[1] 李淑清[1] 肖容辉[1] 

机构地区：[1]青岛理工大学环境与市政工程学院,青岛266033

出　　处：《分析试验室》2009年第3期6-9,共4页Chinese Journal of Analysis Laboratory

基　　金：青岛理工大学引进人才科研启动费(C2007-008);山东省教育厅科技计划(J07WZ05)项目资助

摘　　要：建立了固相萃取-反相高效液相色谱法检测水中3种邻苯二甲酸酯类物质邻苯二甲酸二甲酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯的方法。考察了固相萃取柱、洗脱溶剂、洗脱体积、上样速度以及洗脱速度对萃取效率的影响。通过综合分析,选定SupelcleanLC-18 SPE Tube固相萃取柱,甲醇为洗脱剂,洗脱体积2mL,上样速度为4mL/min,洗脱速度为1mL/min。在此萃取条件下,萃取回收率在83.4%～121.2%之间。邻苯二甲酸二甲酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯质量浓度在2～100mg/L之间均为线性。经萃取后,方法的最低检出限分别为邻苯二甲酸二甲酯0.06μg/L,邻苯二甲酸二(2-乙基己基)酯0.16μg/L,邻苯二甲酸二正辛酯0.08μg/L。方法的精密度在10%～15%之间。应用该方法测定自来水中酞酸酯类化合物的含量,加标回收率为83.6%～110.2%。Phthalate esters are the suspected endocrine disrupters. These compounds commonly called endocrine dismpter chemicals, are widely used as plastic additives and can be usually found in environmental samples. The simuhaneous determination method of three kinds of phthalic acid esters in tap water, dimethyl o-phthalate （DMP）, di（2-ethylhexyl）o-phthalate （DEHP）, di-n-octyl o-phthalate （DOP）, is proposed by solid phase extraction-reversed phase high performance liquid chromatography. The five main influencing factors on recovery, that is, solid phase extraction column, elution solvent, elution volume, sampling speed and elution speed were studied. A solid-phase extraction with supelclean LC-18 cartridges was carried out and the elution was performed with methanol. Elution speed was 4 mL/min. Sampling speed was 1 mL/min. Under this experiment conditions, the recoveries of extraction were 83.4% 121.2%. All of the linear ranges were 2 - 100 mg/L for DMP, DEHP, DOP. After extraction, the detection limits were 0.06μg/L for DMP, 0.16 μg/L for DEI-IP, 0.08μg/L for DOP, respectively. The RSDs were in the range of 10%- 15%. Recoveries for spiked samples were between 83.6% and 110.2%. The method was validated using standard addition calibration and recovery assays.

关 键 词：固相萃取 高效液相色谱 邻苯二甲酸二甲酯 邻苯二甲酸二正辛酯 邻苯二甲酸二(2-乙基己基)酯 水 

分 类 号：O657.7[理学—分析化学]