Abstract A simple and green procedure was proposed for the separation and preconcentration of ionizable analytes from complex solid-phase samples. The developed procedure was applied to the HPLC–MS/MS determination of two nonsteroidal anti-inflammatory drugs (ketoprofen and diclofenac) in beef liver samples. The procedure included two stages. The first one assumed separation of analytes from a liver sample in a sodium carbonate solution (pH 11). In this case analytes ionization promoted mass-transfer from solid sample phase to alkaline aqueous phase. The second one assumed an effervescence-assisted dispersive liquid–liquid microextraction based on deep eutectic solvent decomposition in alkaline aqueous sample phase resulting extragent and proton donor agent formation. As result, a simple effervescent reaction between proton donor agent and effervescent agent (sodium carbonate) produced carbon dioxide and assisted in a dispersion of extragent. Deep eutectic solvent consisting of menthol and formic acid (1:40 mol) provided excellent extraction of ketoprofen and diclofenac. LODs calculated from a blank test, based on 3σ, were 0.1 and 0.3 μg kg−1 for ketoprofen and diclofenac, respectively.

中文翻译：

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基于低共熔溶剂分解的泡腾辅助分散液液微萃取：测定肝脏中的酮洛芬和双氯芬酸

摘要 提出了一种从复杂固相样品中分离和预浓缩可电离分析物的简单绿色程序。将开发的程序应用于牛肝样品中两种非甾体抗炎药（酮洛芬和双氯芬酸）的 HPLC-MS/MS 测定。该过程包括两个阶段。第一个假设在碳酸钠溶液 (pH 11) 中从肝脏样品中分离分析物。在这种情况下，分析物电离促进了从固体样品相到碱性水相的质量转移。第二个假设基于碱性水样相中的深度共晶溶剂分解导致提取剂和质子供体试剂形成的泡腾辅助分散液-液微萃取。结果，质子供体剂和泡腾剂（碳酸钠）之间的简单泡腾反应产生二氧化碳并有助于提取剂的分散。由薄荷醇和甲酸 (1:40 mol) 组成的低共熔溶剂提供了对酮洛芬和双氯芬酸的出色萃取。根据空白试验计算的 LOD，基于 3σ，酮洛芬和双氯芬酸的 LOD 分别为 0.1 和 0.3 μg kg-1。