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Tandem air-agitated liquid-liquid microextraction as an efficient method for determination of acidic drugs in complicated matrices

机译:串联空气搅拌液-液微萃取是测定复杂基质中酸性药物的有效方法

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A rapid and simple microextraction method with a high sample clean-up, termed as tandem air-agitated liquid-liquid microextraction (TAALLME), is described. This method is based upon the tandem implementation of the air-agitated liquid-liquid microextraction (AALLME), and this approach improves the applicability of the dispersive liquid-liquid microextraction (DLLME) methods in complicated matrices. With very simple tools, the three non-steroidal anti-inflammatory drugs diclofenac, ibuprofen, and mefenamic acid were efficiently extracted, with an overall extraction time of 7 min. By performing the first AALLME, these acidic analytes, contained in an aqueous sample solution (donor phase, 8.0 mL), were extracted into the organic solvent (1,2-dichloroethane, 37 mu L), and their simple back-extraction into the aqueous acceptor solution (pH, 10.01, 51 mu L) was obtained in 2 min by a second implementation of AALLME. Response surface methodology (RSM) was used for optimization of the experimental parameters. The pH values 2.94 and 10.01 were obtained for the donor and acceptor phases, respectively, and the volumes 99.5 and 51 mu L were obtained for the organic solvent and the acceptor phase, respectively, as the optimal extraction conditions. Under the optimized conditions, tandem AALLME-HPLC-UV provided a good linearity in the range of 0.5-4000 ng mL(-1), limits of detection (0.1-0.3 ng mL(-1)), extraction repeatabilities (relative standard deviations (RSDs) below 7.7%, n = 5), and the enrichment factors (EFs) of 80-104. Finally, the applicability of the proposed method was evaluated by the extraction and determination of the drugs under study in the wastewater and human plasma samples. (C) 2016 Elsevier B.V. All rights reserved.
机译:描述了一种快速简单的具有高样品净化率的微萃取方法,称为串联空气搅拌液-液微萃取(TAALLME)。该方法基于空气搅拌液-液微萃取(AALLME)的串联实现,并且该方法提高了分散液-液微萃取(DLLME)方法在复杂基质中的适用性。使用非常简单的工具,可以有效地提取三种非甾体类抗炎药双氯芬酸,布洛芬和甲芬那酸,总提取时间为7分钟。通过执行第一个AALLME,将样品水溶液(供体相,8.0 mL)中包含的这些酸性分析物萃取到有机溶剂(1,2-二氯乙烷,37μL)中,并将其简单地反萃取到通过第二次实施AALLME,在2分钟内获得了受体水溶液(pH,10.01,51μL)。响应面法(RSM)用于优化实验参数。作为最佳萃取条件,供体相和受体相的pH值分别为2.94和10.01,有机溶剂相和受体相的体积分别为99.5和51μL。在优化的条件下,串联的AALLME-HPLC-UV在0.5-4000 ng mL(-1),检测限(0.1-0.3 ng mL(-1)),提取重复性(相对标准偏差)范围内提供了良好的线性。 (RSDs)低于7.7%,n = 5),富集因子(EFs)为80-104。最后,通过提取和测定废水和人体血浆样品中正在研究的药物,评估了该方法的适用性。 (C)2016 Elsevier B.V.保留所有权利。

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