色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-衍生化气相色谱/质谱法测定制药厂污水中的环境雌激素

黄成,姜理英,陈建孟,陈效   

  1. Department of Biological and Environmental Engineering, Zhejiang University of Technology, Hangzhou 310014, China
  • 收稿日期:2008-10-27 修回日期:2008-10-27 出版日期:2008-10-27 发布日期:1983-09-25
  • 通讯作者: 姜理英
  • 基金资助:

Determination of environmental estrogens in pharmacy wastewater using solid-phase extraction-gas chromatography/mass spectrometry with derivatization

HUANG Cheng, JIANG Liying, CHEN Jianmeng, CHEN Xiao   

  1. Department of Biological and Environmental Engineering, Zhejiang University of Technology, Hangzhou 310014, China
  • Received:2008-10-27 Revised:2008-10-27 Online:2008-10-27 Published:1983-09-25
  • Contact: JIANG Liying

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摘要： 采用固相萃取-衍生化气相色谱/质谱法(GC/MS)测定某制药厂污水中的雌酮(E1)、雌二醇(E2)、雌三醇(E3)和乙炔基雌二醇(EE2)4种雌激素化合物。样品经固相萃取柱萃取富集及双(三甲基硅烷基)三氟乙酰胺(1%三甲基氯硅烷)（BSTFA(1%TMCS)）衍生化后进行GC/MS分析。该法对4种目标物的检出限为1.8～4.7 ng/L,相对标准偏差为2.3%～9.1%(n=8)。目标化合物的加标回收率为（94.0±2.9）%～（101±3.8）%,说明该方法能较好地应用于污水中雌激素化合物的定量检测。通过对某制药厂污水中的雌激素进行定量分析,发现污水中乙炔基雌二醇和雌酮质量浓度分别达396.6 和39.9 ng/L；经过传统的厌氧兼氧好氧生物处理后,污水中的环境雌激素的去除率仅为35%～40%,说明传统的污水处理工艺对去除污水中雌激素效果并不明显，需要改进。

关键词: 固相萃取, 环境雌激素, 气相色谱/质谱法, 污水 , 衍生化

Abstract: A method for the determination of estrone (E1), estradiol (E2), ethinylestradiol (EE2) and estriol (E3) in pharmacy wastewater was developed using solid-phase extraction-gas chromatography/mass spectrometry （SPE-GC/MS） with derivatization. The sample was extracted by an SPE column, derivatized by bis(trimethylsilyl) rifluoroacetamide （BSTFA）, and analyzed by GC/MS. The detection limits were 1.8-4.7 ng/L, and the relative standard deviations were 2.3%-9.1% (n=8). The recoveries of above four environmental estrogen compounds were (94.0±2.9)% to (101±3.8)%. The method can be applied in the determination of the estrogenic compounds in wastewater samples successfully. The concentrations of EE2 and E1 in wastewater were 396.6 ng/L and 39.9 ng/L, respectively, and the removal rates of EE2 and E1 were 35%-40% after traditional biological treatment. The results demonstrated that the removal efficiency was not satisfactory and the traditional treatment process of wastewater containing estrogen compounds from pharmaceaticals factory should be improved.

Key words: derivatization, environmental estrogens, gas chromatography/mass spectrometry (GC/MS), wastewater , solid-phase extraction