固相萃取-气质联用测定水中的邻苯二甲酸酯

Determination of phthalate acid esters in water by solid-phase extraction and GC-MS

为建立水中邻苯二甲酸酯(Phthalic acid esters,PAEs)固相萃取-气相色谱质谱法测定体系,以应用于珠江广州段水体中邻苯二甲酸酯的测定.从洗脱剂种类、水样pH值和洗脱剂体积等方面优化固相萃取条件,采用气相色谱—质谱法对水中邻苯二甲酸二甲酯(Dimethyl phthalate,DMP)、邻苯二甲酸二乙酯(Diethyl phthalate,DEP)、邻苯二甲酸二丁酯(Dibutyl phthalate,DBP)及邻苯二甲酸二异辛酯(Diethylhexyl phthalate,DEHP)等4种目标物质进行了定量分析.结果表明:在水样pH值为2.0,以4 mL V(乙酸乙酯)∶V(二氯甲烷)=1∶1为洗脱剂时,4种邻苯二甲酸酯的回收率为65.12%~108.86%;该方法检出限范围为0.05~0.45μg/L,平均回收率为86.11%~105.85%,相对标准偏差为1.77%~4.42%.该法简便、快捷和准确,适用于水中邻苯二甲酸酯含量的测定.

Establishing determination system with solid-phase extraction and gas chromatography mass spectrometry （GC-MS） for application of the determination of phthalatic acid esters （PAEs） in Pearl River of Guangzhou section. Conditions of solid phase extraction were optimized by the type of eluent, pH value of water sample and volume of eluent, GC-MS was used to quantitate and analyze 4 kinds of target materials, such as dimethyl phthalate （DMP）, diethyl phthalate （DEP）, dibutyl phthalate （DBP）, diethylhexyl phthalate （DEHP）. The results showed that, when the pH value of water sample was 2. 0, and 4 mL V （ methylene chloride） ： V （ ethyl acetate ） = 1 ： 1 was used as the eluent, the recovery rate among 4 kinds of phthalic acid esters were 65.12% - 108.86% ; The detection limit ranges were from 0. 05 to 0. 45 μg/L, the average recovery was 86. 11% - 86. 11% , and relative standard deviation was 1.77% -4. 42%. This method is suitable for determining the content of phthalates in water for the advantages of convenience, fast and accuracy.