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固相萃取-衍生化气相色谱/质谱法测定制药废水中的环境雌激素

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

作者信息

Huang Cheng, Jiang Liying, Chen Jianmeng, Chen Xiao

机构信息

Department of Biological and Environmental Engineering, Zhejiang University of Technology, Hangzhou 310014, China.

出版信息

Se Pu. 2008 Sep;26(5):618-21.

PMID:19160764
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) trifluoroacetamide (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 pharmaceuticals factory should be improved.

摘要

建立了一种采用固相萃取-气相色谱/质谱联用(SPE-GC/MS)并衍生化的方法来测定制药废水中的雌酮(E1)、雌二醇(E2)、炔雌醇(EE2)和雌三醇(E3)。样品通过SPE柱萃取,用双(三甲基硅基)三氟乙酰胺(BSTFA)进行衍生化,然后用GC/MS分析。检测限为1.8 - 4.7 ng/L,相对标准偏差为2.3% - 9.1%(n = 8)。上述四种环境雌激素化合物的回收率为(94.0 ± 2.9)%至(101 ± 3.8)%。该方法可成功应用于废水样品中雌激素化合物的测定。废水中EE2和E1的浓度分别为396.6 ng/L和39.9 ng/L,传统生物处理后EE2和E1的去除率为35% - 40%。结果表明去除效率不理想,制药厂含雌激素化合物废水的传统处理工艺应加以改进。

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