首页> 外文期刊>Journal of Residuals Science & Technology >Detection of estrone, 17β-estadiol, 17α-ethynyl estradiol and estrogen-3-sulfate in wastewater and river by Solid Phase Extraction/HPLC-MS/MS
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Detection of estrone, 17β-estadiol, 17α-ethynyl estradiol and estrogen-3-sulfate in wastewater and river by Solid Phase Extraction/HPLC-MS/MS

机译:固相萃取/ HPLC-MS / MS法检测废水和河流中的雌酮,17β-雌二醇,17α-乙炔基雌二醇和3-硫酸雌激素

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Background: Steroid estrogens are the most concerned environmental hormones presented in wastewater at the nano-gram per liter level. Conjugated estrogens are ready to release free estrogens given appropriate environmental conditions thus result in potential environmental risk due to the active property of free ones. Materials and Methods: The analysis of estrogens has been a challenge due to the trace concentration, especially the simultaneous analysis of free and conjugated estrogens. Estrone (E1), 17β-estadiol (E2), 17α-ethynyl estradiol (EE2) and estrogen-3-sulfate (E1-3-S) were simultaneously analyzed using an HPLC-MS-MS preceded by solid phase extraction (SPE) sample pretreatment, and the samples were collected along a typical wastewater treatment train and in the receiving river. Results: The four estrogens were detected in all samples. E1-3-S accounted for 49.4% and 57.3% of E1 and total estrogens in receiving water body samples (in E2 equivalent concentrations). The linear detection ranges for E1; E2; EE2 and E1-3-S are 0.5-100.1 ng/mL, 0.4-98.8 ng/mL, 0.1-99.4 ng/mL and 0.2-100.0 ng/mL; the limits of detection are 0.5; 0.4; 0.1 and 0.2 ng/L respectively. The repeatability and precision is satisfactory; the spiking recovery rate is lower than 85%. The time-lasting for the analysis of a mixed sample is 12.0min. Main conclusions: This research suggested an analysis method which is able to provide reasonable repeatability, precision and recovery with less sample volume, and firstly reported the conjugated estrogen levels along the treatment train in China.
机译:背景:类固醇雌激素是废水中存在的最受关注的环境激素,浓度为纳克每升。在适当的环境条件下,结合的雌激素准备释放游离的雌激素,因此由于游离雌激素的活性而导致潜在的环境风险。材料和方法:由于痕量浓度,尤其是同时分析游离和结合的雌激素时,雌激素的分析一直是一个挑战。使用HPLC-MS-MS同时固相萃取(SPE)同时分析了雌酮(E1),17β-雌二醇(E2),17α-乙炔基雌二醇(EE2)和3-硫酸雌激素(E1-3-S)样品预处理,然后沿着典型的废水处理列车并在接收河中收集样品。结果:所有样品中均检出4种雌激素。 E1-3-S分别占接收水体样品中E1和总雌激素的49.4%和57.3%(以E2当量浓度计)。 E1的线性检测范围; E2; EE2和E1-3-S为0.5-100.1 ng / mL,0.4-98.8 ng / mL,0.1-99.4 ng / mL和0.2-100.0 ng / mL;检出限为0.5; 0.4;分别为0.1和0.2 ng / L。重复性和精度令人满意;峰值恢复率低于85%。混合样品的分析时间为12.0分钟。主要结论:本研究提出了一种能够提供合理的可重复性,精密度和回收率且样品量较少的分析方法,并首先报道了中国沿治疗路线的结合雌激素水平。

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