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,pH=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 pH value of 7 was 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%.
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