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采用新型离子印迹聚合物固相萃取法测定水中、葡萄酒和蜂蜜中的铀。

Uranium Determination in Waters, Wine and Honey by Solid Phase Extraction with New Ion Imprinted Polymer.

机构信息

Faculty of Chemistry and Pharmacy, University of Sofia "St. Kliment Ohridski", 1164 Sofia, Bulgaria.

出版信息

Molecules. 2022 Aug 27;27(17):5516. doi: 10.3390/molecules27175516.

Abstract

An analytical method for uranium determination in waters, wine and honey was developed based on solid phase extraction (SPE) with new ion imprinted polymer. The sorbent was synthesized using 4-(2-Pyridylazo)resorcinol (PAR) as a ligand via dispersion polymerization and characterized by SEM for morphology and shape of polymer particles and nitrogen adsorption-desorption studies for their surface area and total pore volume. The kinetic experiments performed showed that the rate limiting step is the complexation between U(VI) ions and chelating ligand PAR incorporated in the polymer matrix. Investigations by Freundlich and Langmuir adsorption isotherm models showed that sorption process occurs as a surface monolayer on homogeneous sites. The high extraction efficiency of synthesized sorbent toward U(VI) allows its application for SPE determination of U(VI) in wine and honey without preliminary sample digestion using ICP-OES as measurement method. The recoveries achieved varied: (i) between 88 to 95% for surface and ground waters, (ii) between 90-96% for 5% aqueous solution of honey, (iii) between 86-93% for different types of wine. The validity and versatility of proposed analytical methods were confirmed by parallel measurement of U in water samples using Alpha spectrometry and U analysis in wine and honey after sample digestion and ICP-MS measurement. The analytical procedure proposed for U determination in surface waters is characterized with low limits of detection/quantification and good reproducibility ensuring its application for routine control in national monitoring of surface waters. The application of proposed method for honey and wine samples analysis provides data for U content in traditional Bulgarian products.

摘要

基于固相萃取(SPE)和新型离子印迹聚合物,开发了一种用于测定水中、葡萄酒和蜂蜜中铀的分析方法。该吸附剂是通过分散聚合,以 4-(2-吡啶偶氮)间苯二酚(PAR)为配体合成的,并通过 SEM 对聚合物颗粒的形态和形状以及氮气吸附-解吸研究对其表面积和总孔体积进行了表征。动力学实验表明,速率限制步骤是 U(VI)离子与聚合物基质中螯合配体 PAR 之间的络合。Freundlich 和 Langmuir 吸附等温线模型的研究表明,吸附过程是在均匀位上发生的表面单层吸附。合成的吸附剂对 U(VI)的高萃取效率使其能够应用于 SPE 测定葡萄酒和蜂蜜中的 U(VI),而无需使用 ICP-OES 作为测量方法对样品进行预先消化。获得的回收率如下:(i)地表和地下水中的回收率为 88-95%,(ii)5%蜂蜜水溶液中的回收率为 90-96%,(iii)不同类型葡萄酒中的回收率为 86-93%。使用 Alpha 谱法平行测量水样中的 U 以及样品消化后使用 ICP-MS 测量葡萄酒和蜂蜜中的 U 分析,验证了所提出的分析方法的有效性和通用性。用于地表水 U 测定的分析程序具有较低的检测/定量限和良好的重现性,确保其可用于国家地表水常规监测中的常规控制。所提出的方法在蜂蜜和葡萄酒样品分析中的应用为保加利亚传统产品中的 U 含量提供了数据。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6ab3/9457621/4c11b47c309f/molecules-27-05516-g001.jpg

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