Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building (Annex), Campus de Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building (Annex), Campus de Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Talanta. 2015 Jan;131:645-9. doi: 10.1016/j.talanta.2014.08.031. Epub 2014 Aug 20.
In this article, a new homogeneous liquid-liquid microextraction alternative, based on the use of switchable hydrophilicity solvents (SHS), is presented for the first time. The extraction technique makes use of a water-immiscible solvent (N,N-Dimethylcyclohexylamine) that can be solubilised in 1:1 ratio using CO2 as reagent. After the extraction, phases' separation is induced by the addition of sodium hydroxide, which produces a change on the ionisation state of the amine, centrifugation not being necessary. The extraction technique has been optimised and characterised using the determination of benz[a]anthracene by fluorimetric measurements in water samples as model analytical problem. Although the native fluorescence of the compound is quenched in the organic phase, this attenuation is reduced by diluting the extractant (1:1) in acetic acid. The fluorescence intensity is 35% higher in the SHS-acetic acid mixture than that obtained in pure methanol. The proposed method allows the determination of the target analyte with limit of detection of 0.08 μg/L and good precision (relative standard deviation of 6.7% at the limit of quantification level). The recoveries were in the range of 72-100% fulfilling the Environmental Protection Agency criterion. Finally, the potential use of this microextraction technique in combination with gas chromatography is shown for several polycyclic aromatic hydrocarbons.
本文首次提出了一种基于可切换亲水性溶剂 (SHS) 使用的新型均相液-液微萃取替代方法。该萃取技术利用一种与水不混溶的溶剂(N,N-二甲基环己胺),可以与 CO2 以 1:1 的比例溶解。萃取后,通过加入氢氧化钠诱导相分离,这会导致胺的电离状态发生变化,无需进行离心。该萃取技术已通过使用水样品中苯并[a]蒽的荧光光度法测定作为模型分析问题进行了优化和表征。尽管该化合物的固有荧光在有机相中被猝灭,但通过将萃取剂(1:1)稀释在乙酸中,可以减轻这种衰减。在 SHS-乙酸混合物中的荧光强度比在纯甲醇中高 35%。所提出的方法允许以 0.08μg/L 的检测限测定目标分析物,并且具有良好的精密度(在定量限水平下的相对标准偏差为 6.7%)。回收率在 72-100%范围内,符合环境保护局的标准。最后,展示了这种微萃取技术与气相色谱结合在几种多环芳烃中的潜在应用。