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基于1-(邻甲苯基)硫脲的深共熔溶剂作为流动注射分析系统中的固定相用于食用油中汞和铜的测定。

1-(o-Tolyl)thiourea-based deep eutectic solvent as a stationary phase in flow injection analysis system for mercury and copper determination in edible oils.

作者信息

Shishov Andrey, Markova Ulyana, Mulloyarova Valeriia, Tolstoy Peter, Shkaeva Natalya, Kosyakov Dmitry, Das Nipu Kumar, Banerjee Tamal

机构信息

Institute of Chemistry, Saint-Petersburg University, Saint Petersburg State University, SPbSU, SPbU, 7/9 Universitetskaya nab., St. Petersburg, 199034, Russia.

Institute of Chemistry, Saint-Petersburg University, Saint Petersburg State University, SPbSU, SPbU, 7/9 Universitetskaya nab., St. Petersburg, 199034, Russia.

出版信息

Talanta. 2025 Jan 1;282:127079. doi: 10.1016/j.talanta.2024.127079. Epub 2024 Oct 19.

Abstract

In this work, a novel deep eutectic solvent (DES) composed of thymol and 1-(o Tolyl)thiourea 9/1 (mol) is presented for the first time. This DES has not been described in the literature. This DES was first used as a stationary phase in an extraction column integrated into a flow injection analysis system for the simultaneous determination of mercury and copper in edible oils. The automated approach involves passing an aqueous sample solution obtained after microwave mineralization through a microcolumn of DES retained on polytetrafluoroethylene. This leading to the extraction and concentration of the analytes. The metals are then eluted with an aqueous thiourea solution for subsequent analysis by inductively coupled plasma-optical emission spectrometry. The limits of detection (LODs) for mercury and copper were 3 μg L⁻ and 2.5 μg L⁻, respectively. The approach demonstrated high accuracy. Relative standard deviations (RSD) for repeatability and inter-day reproducibility ranged from 3 % to 11 %. Extraction recovery of both metals exceeded 95 %, indicating the high efficiency of the DES-based extraction process. Environmental assessment using the AGREEprep method yielded a favorable environmental index of 0.54, highlighting the robustness of the approach. This novel use of DES as a stationary phase in flow injection analysis system provides a robust, efficient and environmentally friendly approach to the determination of trace metals in edible oils. This method can also be applied to the analysis of other samples.

摘要

在本研究中,首次提出了一种由百里香酚和1-(邻甲苯基)硫脲9/1(摩尔比)组成的新型低共熔溶剂(DES)。该DES在文献中尚未有描述。这种DES首次被用作集成于流动注射分析系统的萃取柱中的固定相,用于同时测定食用油中的汞和铜。该自动化方法包括将微波消解后得到的水样通过保留在聚四氟乙烯上的DES微柱。这导致了分析物的萃取和浓缩。然后用硫脲水溶液洗脱金属,以便随后通过电感耦合等离子体发射光谱法进行分析。汞和铜的检测限(LOD)分别为3 μg L⁻¹和2.5 μg L⁻¹。该方法显示出高准确度。重复性和日间重现性的相对标准偏差(RSD)范围为3%至11%。两种金属的萃取回收率均超过95%,表明基于DES的萃取过程效率很高。使用AGREEprep方法进行的环境评估得出了有利的环境指数0.54,突出了该方法的稳健性。这种将DES用作流动注射分析系统固定相的新用途为食用油中痕量金属的测定提供了一种稳健、高效且环保的方法。该方法也可应用于其他样品的分析。

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