School of Chemistry and Chemical Engineering, University of South China, 28 Changsheng West Road Hengyang, Hunan 421001, PR China.
Talanta. 2010 Apr 15;81(1-2):30-6. doi: 10.1016/j.talanta.2009.11.032. Epub 2009 Nov 17.
A new pyrazole derivative 1-phenyl-3-methylthio-4-cyano-5-acrylicacidcarbamoyl-pyrazole (PMTCAACP) was synthesized and chosen as a complexing monomer for the preparation of surface-grafted ion-imprinted polymers for selective solid-phase extraction of thorium(IV). The silica gel, modified with maleic anhydride, was prepared as a carrier material. In the ion-imprinting process, Th(IV) was complexed with PMTCAACP, and then imprinted in the polymers grafted to the surface of modified silica gel. Subsequently, the template Th(IV) ions were removed with 6 mol/L HCl solution. The obtained ion-imprinted particles for Th(IV) showed specific recognition, and rapid adsorption and desorption kinetics process. The maximum static and total dynamic adsorption capacity of the ion-imprinted polymers (IIPs) for Th(IV) was 64.8 and 37.4 mg/g, respectively. The relative selectivity coefficient values of the imprinted adsorbent for Th(IV)/U(VI), Th(IV)/Ce(III), Th(IV)/La(III), and Th(IV)/Zr(IV) were 72.9, 89.6, 93.8, and 137.2 times greater than non-imprinted matrix, respectively. The interference effect of common cations tested did not interfere with the recovery of Th(IV). The enhancement factor of 20.2, the detection limit of 0.43 microg/L, and the precision of 2.47% (n=7) of the method under the optimized conditions were obtained. Additionally, the calibration curve (r=0.9993) was linear in the range of 1.43-103 microg/L of thorium(IV). The prepared IIPs were shown to be promising for solid-phase extraction coupled with UV-vis spectrophotometry for determination of trace Th(IV) in real samples.
一种新的吡唑衍生物 1-苯基-3-甲基硫代-4-氰基-5-丙烯酰胺基吡唑(PMTCAACP)被合成,并被选为用于制备用于选择性固相萃取钍(IV)的表面接枝离子印迹聚合物的络合单体。硅胶用马来酸酐改性,用作载体材料。在离子印迹过程中,Th(IV)与 PMTCAACP 络合,然后印迹在接枝到改性硅胶表面的聚合物中。随后,用 6 mol/L HCl 溶液除去模板 Th(IV)离子。获得的用于 Th(IV)的离子印迹颗粒表现出特异性识别,以及快速的吸附和解吸动力学过程。离子印迹聚合物(IIP)对 Th(IV)的最大静态和总动态吸附容量分别为 64.8 和 37.4 mg/g。印迹吸附剂对 Th(IV)/U(VI)、Th(IV)/Ce(III)、Th(IV)/La(III)和 Th(IV)/Zr(IV)的相对选择性系数值分别比非印迹基质高 72.9、89.6、93.8 和 137.2 倍。测试的常见阳离子的干扰效应不会干扰 Th(IV)的回收。在优化条件下,该方法的增强因子为 20.2,检测限为 0.43 μg/L,精密度为 2.47%(n=7)。此外,在 1.43-103 μg/L 的钍(IV)范围内,校准曲线(r=0.9993)呈线性。所制备的 IIP 有望与紫外可见分光光度法结合用于固相萃取,以测定实际样品中的痕量 Th(IV)。