Simultaneous determination of four trace estrogens in feces, leachate, tap and groundwater using solid-liquid extraction/auto solid-phase extraction and high-performance liquid chromatography with fluorescence detection.
Simultaneous determination of four trace estrogens in feces, leachate, tap and groundwater using solid-liquid extraction/auto solid-phase extraction and high-performance liquid chromatography with fluorescence detection.
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DOI：
10.1002/jssc.201500443
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发表时间：
2015-10
影响因子：
3.1
通讯作者：
Na Liu;Yue-e Shi;Mengyan Li;Tingdi Zhang;Song Gao
中科院分区：
文献类型：
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作者：
Na Liu;Yue-e Shi;Mengyan Li;Tingdi Zhang;Song Gao
建立了一种同时测定环境基质中4种雌激素（雌酮、雌二醇、雌三醇和17α-乙炔基雌二醇）的高效液相色谱-荧光检测方法。对于粪便样品，使用乙腈和乙酸乙酯的1：1 v/v混合物作为提取溶剂进行固液提取。对于液体样品（例如，渗滤液和地下水），选择疏水/亲脂平衡的自动固相萃取盘，因为与常规C18盘相比，它们具有高回收率。在反相C18柱上进行色谱分离，用乙腈和水的45：55 v/v混合物梯度洗脱。检测限分别为1.1 × 10（-2）（雌酮）、4.11 × 10（-4）（雌二醇）、5.2 × 10（-3）（雌三醇）和7.18 × 10（-3）μg/L在288/310 nm激发/发射波长处测定17α-乙炔基雌二醇，回收率在96.9 ± 3.2-105.4 ± 3.2%（n = 3）之间。该方法已成功地应用于畜禽粪便和水样中雌激素的测定，并在中国东北的一个主要河流。我们观察到相对较高的丰度和广泛分布的所有四种雌激素在我们的样品收集，这意味着在我们的研究领域的雌激素的命运和污染的全面和复杂的调查的紧迫性。
A simple and selective high-performance liquid chromatography method coupled with fluorescence detection was developed for the simultaneous measurement of trace levels of four estrogens (estrone, estradiol, estriol and 17α-ethynyl estradiol) in environmental matrices. For feces samples, solid-liquid extraction was applied with a 1:1 v/v mixture of acetonitrile and ethyl acetate as the extraction solvent. For liquid samples (e.g., leachate and groundwater), hydrophobic/lipophilic balanced automated solid-phase extraction disks were selected due to their high recoveries compared to conventional C18 disks. Chromatographic separations were performed on a reversed-phase C18 column gradient-eluted with a 45:55 v/v mixture of acetonitrile and water. The detection limits were down to 1.1 × 10(-2) (estrone), 4.11 × 10(-4) (estradiol), 5.2 × 10(-3) (estriol) and 7.18 × 10(-3) μg/L (17α-ethynyl estradiol) at excitation/emission wavelengths of 288/310 nm, with recoveries in the range of 96.9 ± 3.2-105.4 ± 3.2% (n = 3). The method was successfully applied to determine estrogens in feces and water samples collected at livestock farms and a major river in Northeast China. We observed relatively high abundance and widespread distribution of all four estrogens in our sample collections, implying the urgency for a comprehensive and intricate investigation of estrogenic fate and contamination in our researched area.