Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia, Dr. Moliner 50, 46100, Burjassot, Valencia, Spain.
Department of Organic Chemistry, Faculty of Chemistry, University of Valencia, Dr. Moliner 50, 46100, Burjassot, Valencia, Spain.
Mikrochim Acta. 2019 Aug 10;186(9):615. doi: 10.1007/s00604-019-3739-4.
A hybrid material made of β-cyclodextrin anchored to a polymeric network is described and evaluated as a sorbent for solid-phase extraction of phenolic compounds (phenol, cresol isomers, 2-methoxy-4-vinylphenol, 4-ethylphenol, 4-vinylphenol, 4-ethylguaiacol, guaiacol, and eugenol). The polymeric backbone of the sorbent consists of a poly(glycidyl-co-ethylene dimethacrylate) network, whose surface has been modified with β-cyclodextrin by a click-chemistry based procedure. The resulting material has been characterized by different techniques, and it has shown to be viable as a sorbent for its use in extraction cartridges. In this way, a method for the determination of the above analytes in tea has been validated. Under optimum conditions, the method has good repeatability, with coefficients of variation between 0.6 and 7.2%. In addition, recoveries from spiked samples at the level of 50 μg L are between 57 and 101%. The method has been then applied to the determination of phenolic compounds in the drinkable portion of infusions made from tea bags. The quantification has been carried out by using gas chromatography coupled to a mass spectrometry detector. Following their elution from the sorbent with a mixture of acetonitrile and methanol, the limits of quantification reached are between 4.6 and 400 μg L. Results have been compared with those obtained with a reference method by using the paired t-test for comparing individual differences. The solid phase is reusable, and no cyclodextrin is lost during extraction due to its covalent anchoring to the polymeric support. Graphical abstract Schematic representation of the structure and characterization of the hybrid material made of β-cyclodextrin anchored to a polymeric network. The material is described and evaluated as a sorbent for the solid-phase extraction of phenolic compounds.
一种由 β-环糊精锚定在聚合物网络上的杂化材料被描述并评估为用于固相萃取酚类化合物（苯酚、甲酚异构体、2-甲氧基-4-乙烯基苯酚、4-乙基苯酚、4-乙烯基苯酚、4-乙基愈创木酚、愈创木酚和丁香酚）的吸附剂。吸附剂的聚合物骨架由聚（缩水甘油基-co-乙二甲基丙烯酸酯）网络组成，其表面通过基于点击化学的程序用 β-环糊精进行了修饰。所得材料已通过不同技术进行了表征，并且已证明其作为吸附剂在萃取小柱中是可行的。通过这种方式，验证了一种用于测定茶中上述分析物的方法。在最佳条件下，该方法具有良好的重复性，变异系数在 0.6%至 7.2%之间。此外，在 50μg L 的水平下从加标样品中的回收率在 57%至 101%之间。然后将该方法应用于测定茶包冲泡饮料中酚类化合物的含量。使用气相色谱-质谱联用仪进行定量分析。在使用乙腈和甲醇混合物从吸附剂中洗脱后，达到的定量限在 4.6 至 400μg L 之间。使用配对 t 检验比较个体差异，将结果与参考方法进行了比较。固相可重复使用，并且由于其与聚合物载体的共价结合，在萃取过程中不会损失环糊精。
