Thermo-Assisted Deep Eutectic Solvent Based on Dispersive Liquid-Liquid Microextraction for Preconcentration of Phthalate Esters in Water Samples and Determination by Gas Chromatography With Flame Ionization Detection
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引用次数: 0
Abstract
A thermo-assisted deep eutectic solvent (DES) based on dispersive liquid-liquid microextraction followed by gas chromatography with flame ionization detection was developed for the analysis of five phthalate esters in different water samples. In the procedure involved, a DES composed of lidocaine, an amphiphilic amine, and oleic acid, was mixed with the sample assisted by ultrasound, and phase separation was achieved with increasing temperature. The heating of the extraction system induced the change of acid-base properties of the DES components. Thus, the formation of microdroplets of DES in the sample was provided, and two phases were separated. The structure of the upper hydrophobic layer was characterized by Fourier-transform infrared spectroscopy. Also, the amount of water in the DES phase was analyzed by mass spectrometer and Karl Fischer titration. Some critical variables on the extraction yield were assessed. The proposed method achieved 1.2–1.3 and 4.1–4.3 µg/L for limits of detection and limits of quantification, respectively. The intra-day and inter-day percentage relative standard deviations (n = 5) were determined to be in the range of 4.2–6.2% and 5.1–7.2%, respectively. Ultimately, this method analyzed the five phthalate esters in different water samples with high recoveries.
为分析不同水样中的五种邻苯二甲酸酯,开发了一种基于分散液-液微萃取的热辅助深共晶溶剂(DES),然后采用气相色谱法进行火焰离子化检测。在该方法中,由利多卡因、两性胺和油酸组成的 DES 在超声波的辅助下与样品混合,并随着温度的升高实现相分离。萃取系统的加热引起了 DES 成分酸碱性质的变化。因此,样品中的 DES 形成了微滴,并分离出两相。通过傅立叶变换红外光谱法对上层疏水层的结构进行了表征。此外,还利用质谱仪和卡尔费休滴定法分析了 DES 相中的含水量。对萃取率的一些关键变量进行了评估。该方法的检出限和定量限分别为 1.2-1.3 微克/升和 4.1-4.3 微克/升。日内和日间相对标准偏差(n = 5)分别为 4.2-6.2% 和 5.1-7.2%。最终,该方法以较高的回收率分析了不同水样中的五种邻苯二甲酸酯。
期刊介绍:
The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.