Dispersive liquid-liquid microextraction with solidification of floating organic drop combined with high performance liquid chromatography for the determination of phenolic oestrogens from human urine and water samples
Dispersive liquid-liquid microextraction with solidification of floating organic drop combined with high performance liquid chromatography for the determination of phenolic oestrogens from human urine and water samples
复制标题
分散液-液微萃取与漂浮有机液滴固化结合高效液相色谱法测定人尿和水样中的酚类雌激素
DOI：
10.1080/03067319.2019.1597869
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发表时间：
2019
影响因子：
2.6
通讯作者：
Wen Yingying
中科院分区：
文献类型：
--
作者：
Niu Zongliang;Zhang Jun;Wu Dongming;Wen Yingying
建立了一种新的、简单、快速的分散液-液微萃取-高效液相色谱法测定人尿和水样中己烯雌酚、己烯雌酚和己雌酚的方法。优化了悬浮有机液滴固化分散液-液微萃取过程中样品pH值、分散剂种类和体积、萃取剂种类和体积等参数。采用高效液相色谱法对酚类雌激素进行分析。在优化的萃取和检测条件下，获得了良好的分析性能。己烯雌酚和双烯雌酚的峰面积与浓度之间的良好线性关系（r≥ 0.998）在0.1 - 20 µg/mL范围内优化，己烷雌酚在2 - 50 µg/mL范围内优化。方法检出限为28.6-666.7 ng/mL。尿、湖水和自来水样品的相对回收率在72%~ 122%之间，相对标准偏差（RSD，n = 6）在1.5%~ 9.8%之间。所建立的有机悬浮液滴固化分散液液微萃取-高效液相色谱法在生物样品和水样中痕量酚类雌激素残留分析中具有很大的应用潜力。
A novel, simple and rapid method, termed dispersive liquid–liquid microextraction with solidification of floating organic drop coupled to high performance liquid chromatography, was developed for analysis of three phenolic oestrogens including diethylstilbestrol, dienestrol and hexestrol in human urine and water samples. The parameters of dispersive liquid–liquid microextraction with solidification of floating organic drop procedure including sample pH, type and volume of disperser solvent, and type and volume of extraction solvent were optimised. High performance liquid chromatography was applied for the phenolic oestrogens’ analysis. Under the optimum extraction and detection conditions, excellent analytical performances were attained. Good linear relationships (r≥ 0.998) between peak area and concentration for diethylstilbestrol and dienestrol were optimised from 0.1 to 20 µg/mL, for hexestrol from 2 to 50 µg/mL. Method detection limits of 28.6–666.7 ng/mL were achieved. Satisfactory relative recoveries ranging from 72% to 122% were determined for urine, lake and tap water samples, with relative standard deviations (RSDs, n = 6) of 1.5–9.8%. The developed dispersive liquid–liquid microextraction with solidification of floating organic drop-high performance liquid chromatography method has a great potential in routine residual analysis of trace phenolic oestrogens in biological and water samples.