气相色谱-质谱联用法同时测定污水中对羟基苯甲酸酯和甾体雌激素  

Simultaneous determination of parabens and steroid estrogens in sewage water using gas chromatography-mass spectrometry

作　　者：王亮[1,2] 毛茜慧 袁守军[1] 黄德英[3] 张继彪[2] 

机构地区：[1]合肥工业大学土木与水利工程学院,合肥230009 [2]复旦大学环境科学与工程系,上海200433 [3]复旦大学化学系,上海200433

出　　处：《环境化学》2016年第1期49-56,共8页Environmental Chemistry

基　　金：上海市自然科学基金(12ZR1440900);高等学校博士学科点专项科研基金(20120071120033)资助~~

摘　　要：利用气相色谱-质谱联用仪(GC-MS),结合固相萃取技术,建立了同时测定污水中7种对羟基苯甲酸酯和5种甾体雌激素的定量分析方法.结果表明,目标物在40℃衍生化反应60 min可达最佳衍生化效果;最佳萃取剂净化条件为:使用HC-C18型SPE柱,p H=7条件下萃取,洗脱液为乙酸乙酯∶丙酮(1∶1,V∶V).该方法检出限(LOD)为1.8—5.7 ng·L-1,线性范围20—2000 ng·L-1(r>0.990),除少量目标物回收率稍高外,大部分目标物的回收率为82.2%—128.5%,相对标准偏差介于4.4%—21.2%之间.A method was developed for the simultaneous detamination of seven parabens and five steroid estrogens in sewage water using gas chromatography-mass spectrometry coupled by solid phase extraction. The sample derivatization was optimized and the best derivatization was obtained when target compounds reacted with bis（ trimethylsilyl） trifluoroacetamide at 40 ℃ for 60 min. The optimum extraction conditions were as follow： HC-C18 cartridge was selected and the p H value of 7was optimized for samples extraction,then ethyl acetate： acetone（ 1∶1,V ∶ V） was used for elution.Under the optimized conditions,the linear detection range of 12 analytes was 20—2000 ng·L-1（ r〉0.990）. The limit of detection was 1.8—5.7 ng·L-1,and the recovery of 82.2-128.5% was obtained for most of the analytes,and the relative standard deviation was 4.4%—21.2%.

关 键 词：气相色谱-质谱法 对羟基苯甲酸酯 甾体雌激素 固相萃取 污水. 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]