Co-precipitation assisted cloud point extraction coupled with high performance liquid chromatography for the determination of estrogens in water and cosmetic samples

Co-precipitation assisted cloud point extraction coupled with high performance liquid chromatography for the determination of estrogens in water and cosmetic samples
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共沉淀辅助浊点萃取结合高效液相色谱法测定水和化妆品样品中的雌激素

DOI:
10.1039/c3ay41372a
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发表时间:
2013-10
期刊:
影响因子:
3.1
通讯作者:
Li Gongke
Li Gongke
中科院分区:
化学3区
文献类型:
--
作者:
Xu Xianfang;Xu Xianfang;Li Gongke;Li Gongke

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建立了一种快速高效的共沉淀辅助浊点提取法,用于环境水样和碳粉中5种雌激素[17β-雌二醇(E_2)、雌酮(E_1)、乙基雌二醇(EE)、己烯雌酚(DES)和己烯雌酚(DHS)]的提取。采用氢氧化铝共沉淀法和十二烷基硫酸钠浊点萃取法相结合的方法提取雌激素。考察了氢氧化铝和十二烷基硫酸钠的浓度、萃取时间、混合类型等因素对目标分析物提取的影响。在最佳条件下,E_2、EE、E_1、DES和DHS的富集倍数分别为31.7、38.5、28.2、40.8和79.5。建立了共沉淀辅助浊点萃取-高效液相色谱法,方法的检出限为0.2~0.7μg L−1,用于环境水样和碳粉中痕量雌激素的测定,回收率为77.3%~104.1%,相对标准偏差为2.0%~10.4%。并与文献报道的方法进行了比较,并对提取机理进行了探讨。该方法快速、灵敏,适用于微量雌激素的分析。
A rapid and efficient co-precipitation assisted cloud point extraction is proposed for extraction of five estrogens [17β-estradiol (E2), estrone (E1), ethinyl estradiol (EE), diethyl stilbestrol (DES) and dihydro stilbestrol (DHS)] in environmental water and toner samples prior to high performance liquid chromatography analysis. It is based on the combination of co-precipitation with aluminum hydroxide and cloud point extraction with sodium dodecylsulfate to extract the target estrogens. Parameters affecting the extraction of target analytes including the concentration of aluminum hydroxide and sodium dodecylsulfate, extraction time, and blending types were investigated. Under optimum conditions, the enrichment factors were 31.7, 38.5, 28.2, 40.8 and 79.5 for E2, EE, E1, DES and DHS, respectively. A co-precipitation assisted cloud point extraction/high performance liquid chromatography method was developed and the limits of detection (LODs) were in the range of 0.2–0.7 μg L−1. The proposed method was successfully applied for the determination of trace estrogens in environmental water and toner samples, and the recoveries ranging from 77.3 to 104.1% with RSD of 2.0–10.4% were obtained. Moreover, the present method was compared to the previously reported methods and the extraction mechanism was also discussed. The method was rapid, sensitive and suitable for the trace estrogen analysis.
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