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以四溴双酚 A 为虚拟模板制备中空多孔分子印迹聚合物及其作为 SPE 吸附剂在测定自来水中双酚 A 中的应用。

Preparation of a hollow porous molecularly imprinted polymer using tetrabromobisphenol A as a dummy template and its application as SPE sorbent for determination of bisphenol A in tap water.

机构信息

Department of Chemistry, University of Science and Technology of China, Hefei 230026, PR China.

出版信息

Talanta. 2013 Dec 15;117:281-7. doi: 10.1016/j.talanta.2013.09.022. Epub 2013 Sep 25.

Abstract

In this paper, a highly selective sample cleanup procedure combing dummy molecular imprinting and solid-phase extraction (DMIP-SPE) was developed for the isolation and determination of bisphenol A (BPA) in tap water. The novel hollow porous dummy molecularly imprinted polymer (HPDMIP) was prepared adopting a sacrificial support approach, using tetrabromobisphenol A (TBBPA), whose structure was similar to that of BPA, as the dummy template and mesoporous MCM-48 nanospheres as the support. Owing to a very short distance between the binding sites and the surface, a large surface area and a good steric structure to match its imprint molecules, the maximum adsorption capacities (Qmax) of the dummy-imprinted and non-imprinted sorbents for BPA were as high as 445 and 340 μmol g(-1), respectively, and the adsorption reached about 73% of Qmax in 10 min. Meanwhile, a method was developed for the determination of BPA using HPDMIP as a solid-phase extraction enrichment sorbent coupled with HPLC. Under the optimum experimental conditions, HPDMIP exhibited satisfactory results in the enrichment and determination of BPA in tap water with a recovery rate of 95-105%, and relative standard deviations of below 6%, and it can achieve a limit of detection as low as 3 ng mL(-1). The developed extraction protocol eliminated the effect of template leakage on quantitative analysis and could be applied for the determination of BPA in complicated functional samples.

摘要

本文开发了一种高度选择性的样品净化程序,结合虚拟分子印迹和固相萃取(DMIP-SPE),用于分离和测定自来水中的双酚 A(BPA)。采用牺牲支撑法制备了新型中空多孔虚拟分子印迹聚合物(HPDMIP),以结构类似于 BPA 的四溴双酚 A(TBBPA)为虚拟模板,介孔 MCM-48 纳米球为支撑。由于结合位点和表面之间的距离非常短,因此具有较大的表面积和良好的空间结构以匹配其印迹分子,虚拟印迹和非印迹吸附剂对 BPA 的最大吸附容量(Qmax)分别高达 445 和 340 μmol g(-1),并且在 10 分钟内吸附达到 Qmax 的约 73%。同时,开发了一种使用 HPDMIP 作为固相萃取富集吸附剂结合 HPLC 测定 BPA 的方法。在最佳实验条件下,HPDMIP 对自来水中 BPA 的富集和测定表现出令人满意的结果,回收率为 95-105%,相对标准偏差低于 6%,检测限低至 3ng mL(-1)。开发的萃取方案消除了模板泄漏对定量分析的影响,并可用于复杂功能样品中 BPA 的测定。

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