Laboratory of Bioanalytical Chemistry, Department of Analytical Chemistry, University of Torino, via Giuria 5, 10125, Turin, Italy.
Anal Bioanal Chem. 2010 May;397(2):815-22. doi: 10.1007/s00216-010-3591-1. Epub 2010 Mar 12.
Superporous monolithic hydrogels (cryogel monoliths) are elastic, sponge-like materials that can be prepared in an aqueous medium through a cryotropic gelation technique. These monoliths show interesting properties for the development of high-throughput solid-phase extraction supports to treat large volumes of aqueous samples. In this work, a cryogel-supported molecularly imprinted solid-phase extraction approach for the endocrine disruptor bisphenol A (BPA) from river water and wine samples is presented. An imprinted polymer with molecular recognition properties for BPA was prepared in acetonitrile by thermal polymerization of a mixture of 4,4'-dihydroxy-2,2-diphenyl-1,1,1,3,3,3-trifluoropropane as a mimic template of BPA, 4-vinylpyridine and trimethylolpropane trimethacrylate in a molar ratio of 1 + 6 + 6. Fine imprinted particles (<10 microm) were embedded in a poly-acrylamide-co-N,N'-methylenbisacrylamide cryogel obtained by ammonium persulfate-induced cryopolymerization at -18 degrees C. The resulting monolithic gel was evaluated for its use as a sorbent support in an off-line solid-phase extraction approach to recover BPA from dilute aqueous samples with minimum pre-loading work-up. The optimized extraction protocol resulted in a reliable MISPE method suitable to selectively extract and preconcentrate BPA from river water and red wine samples, demonstrating the practical feasibility of cryogel-trapped imprinted polymers as solid-phase extraction materials.
超多孔整体水凝胶（冰晶状水凝胶）是具有弹性的海绵状材料，可通过低温凝胶化技术在水性介质中制备。这些整体水凝胶在开发高通量固相萃取支持物方面具有有趣的特性，可用于处理大量水性样品。在这项工作中，提出了一种用于从河水和葡萄酒样品中提取内分泌干扰物双酚 A（BPA）的基于冰晶的印迹固相萃取方法。通过在乙腈中热聚合模拟 BPA 的模板 4,4'-二羟基-2,2-二苯基-1,1,1,3,3,3-三氟丙烷、4-乙烯基吡啶和三羟甲基丙烷三甲基丙烯酸酯，以 1+6+6 的摩尔比制备具有分子识别性能的印迹聚合物。将细小的印迹颗粒（<10 微米）嵌入到在-18°C 下通过过硫酸铵引发的低温聚合获得的聚丙烯酰胺-co-N,N'-亚甲基双丙烯酰胺冰晶中。所得整体凝胶作为吸附剂用于从稀水溶液中离线固相萃取 BPA 的方法进行评估，无需进行最小的预加载工作。优化的萃取方案产生了一种可靠的 MISPE 方法，适用于从河水和红酒样品中选择性提取和预浓缩 BPA，证明了冰晶捕获印迹聚合物作为固相萃取材料的实际可行性。
