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Abstract：
This paper presents a novel dispersive liquid-liquid microextraction (DLLME) method that employs solidified hydrophobic deep eutectic solvent (DES) with hydrophilic DES acting as the dispersant. The aim is to enrich polychlorinated biphenyls (PCBs) from water samples for subsequent determination by gas chromatography-mass spectrometry. The effects of both the hydrophobic DES as the extractant and the hydrophilic DES as the dispersant were thoroughly investigated. Optimization of the key factors influencing extraction efficiency was performed, and the method was subsequently validated. Specifically, a hydrophobic DES called DES2, prepared by combining thymol and decanoic acid in a molar ratio of 3:2, was selected as the extraction solvent. Meanwhile, a hydrophilic DES named DES6, prepared from choline chloride and acetic acid in a molar ratio of 1:2, was chosen as a dispersant. Under the optimal extraction conditions, the developed method exhibited excellent linearity over the concentration range of 0.01-5.0 µg/L, low limits of detection ranging from 3.0 to 5.1 ng/L, relative standard deviations less than 4.1%, and enrichment factors between 182 and 204 for PCBs. Finally, the effectiveness of the developed method was successfully demonstrated through residue determination of PCBs in water samples.
摘要：
本文介绍了一种新型的分散液-液微萃取（DLLME）方法，该方法采用固化的疏水性深共熔溶剂（DES），亲水性DES作为分散剂。目的是从水样中富集多氯联苯（PCBs），以便通过气相色谱-质谱法进行后续测定。彻底研究了疏水性DES作为萃取剂和亲水性DES作为分散剂的效果。对影响提取效率的关键因素进行了优化,随后对该方法进行了验证。具体来说,通过将百里酚和癸酸以3:2的摩尔比组合制备的称为DES2的疏水性DES被选择作为提取溶剂。同时,选择由氯化胆碱和乙酸以1:2的摩尔比制备的名为DES6的亲水性DES作为分散剂。在最佳提取条件下,所开发的方法在0.01-5.0µg/L的浓度范围内表现出优异的线性，检测下限为3.0至5.1ng/L，相对标准偏差小于4.1%，多氯联苯的富集系数在182到204之间。最后,通过对水样中多氯联苯的残留测定，成功证明了该方法的有效性。
