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Orthogonal array design optimisation of an in situ ionic liquid dispersive liquid–liquid microextraction for the detection of phenol and endocrine-disrupting phenols in aqueous samples
Journal of the Iranian Chemical Society ( IF 2.2 ) Pub Date : 2019-11-22 , DOI: 10.1007/s13738-019-01816-x
I. Nowak , I. Rykowska , J. Ziemblińska-Bernart

In this paper, a dispersive liquid–liquid microextraction (DLLME) based on the application of in situ ionic liquids (in situ ionic liquid DLLME) was developed for preconcentration and determination of trace amount of phenol and endocrine-disrupting phenols in aqueous samples. The experimental parameters of an in situ ionic liquid DLLME method were investigated and optimised using an orthogonal array design. Several factors affecting extraction efficiency, including percentage concentration of the ionic liquid, the ratio of ionic liquid to the ion exchanger, extraction time as well as centrifugation time, were investigated and optimised. Under the optimal conditions, percentage concentration of the ionic liquid of 5%, the ratio of ionic liquid to the ion exchanger of 1–2, the extraction time of 5 min and centrifugation time of 1 min, the method affords satisfactory recoveries in the range of 99–100%. Consistent repeatability (RSD ≤ 5%) with satisfactory linearity (0.9993 ≥ r2 ≤ 0.9999) of results illustrated a good performance of the present method. The method was applied to the determination of endocrine-disrupting phenols in real seawater samples. The relative recovery of spiked, natural seawater samples was higher than 97%.

中文翻译:

用于水样品中苯酚和干扰内分泌酚的原位离子液体分散液-液微萃取的正交阵​​列设计优化

本文基于原位离子液体(原位离子液体DLLME)的应用开发了一种分散液-液微萃取(DLLME),用于水溶液中痕量苯酚和干扰内分泌酚的预浓缩和测定。使用正交阵列设计研究并优化了原位离子液体DLLME方法的实验参数。研究和优化了影响萃取效率的几个因素,包括离子液体的浓度百分比,离子液体与离子交换剂的比例,萃取时间以及离心时间。在最佳条件下,离子液体的百分比浓度为5%,离子液体与离子交换剂的比例为1-2,提取时间为5分钟,离心时间为1分钟,该方法的回收率令人满意,范围为99-100%。一致的重复性(RSD≤5%)和令人满意的线性度(0.9993≥ [R 2 结果≤0.9999)中所示的本发明的方法的良好的性能。该方法用于实际海水样品中干扰内分泌酚的测定。加标的天然海水样品的相对回收率高于97%。
更新日期:2019-11-22
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