全自动固相膜萃取-气相色谱-质谱法测定水样中邻苯二甲酸酯

Determination of Phthalate Esters in Water Samples by Automatic Solid-phase Extraction Disk and Gas Chromatography-Mass Spectrometry

本文采用全自动固相膜萃取-气相色谱-质谱联用技术,对水环境中6种邻苯二甲酸酯类有机污染物进行萃取及测定。通过调节萃取水样的pH值、空白控制、固相萃取膜片和洗脱溶剂选择等方式对方法进行了优化和验证。同时对固相萃取水中邻苯二甲酸酯所遇到的常见问题提出了解决方案。水样体积在250 mL时,检出限为0.01~0.12μg/L,空白水样的加标实验中,邻苯二甲酸酯的回收率可达到80.9%~124.0%。除此之外,还对地表水、生活污水和工业废水等实际水样进行了加标回收实验,回收率在73%~132%之间,取得了良好的分析测试效果。

The phthalates esters(PAEs)in water were analyzed by automatic disk solid-phase extraction and gas chromatography-mass spectrometry.The method was optimized by adjusting the pH value of the extracted water sample,blank control,solid phase extraction(SPE)membrane and elution solvent selection.At the same time,the common problems of phthalate extraction by SPE from water were discussed and solved.The recovery was 80.9%-124%for both compounds in distilled water.The limits of detection of the method was between 0.01 and 0.12μg/L in 250 mL water.In addition,recoveries and method precision of phthalates were measured in surface water,sanitary sewage and wastewater.