Departamento de Medio Ambiente, INIA, Carretera de A Coruña km 7.5, 28040 Madrid, Spain.
J Chromatogr A. 2011 Oct 7;1218(40):7065-70. doi: 10.1016/j.chroma.2011.07.092. Epub 2011 Aug 6.
In this paper, a novel format for selective solid-phase extraction based on a molecularly imprinted polymer (MIP) is described. A small amount of MIP has been synthesized within the pores of commercial polyethylene (PE) frits and attached to its surface using benzophenone (BP), a photo-initiator capable to start the polymerisation from the surface of the support material. Key properties affecting the obtainment of a proper polymeric layer, such as polymerisation time and kind of cross-linker were optimised. The developed imprinted material has been applied as a selective sorbent for cleaning extracts of thiabendazole (TBZ), as model compound, from citrus samples. The use of different solvents for loading the analyte in the imprinted frits was investigated, as well as the binding capacity of the imprinted polymer. Imprinted frits showed good selectivity when loads were performed using toluene and a linear relationship was obtained for the target analyte up to 1000 ng of loaded analyte. Prepared composite material was applied to the SPE of TBZ in real samples extracts, showing an impressive clean-up ability. Calibrations showed good linearity in the concentration range of 0.05-5.00 μg g(-1), referred to the original solid sample, and the regression coefficients obtained were greater than 0.996. The calculated detection limit was 0.016 μg g(-1), low enough to satisfactory analysis of TBZ in real samples. RSDs at different spiking levels ranged below 15% in all the cases and imprinted frits were reusable without loss in their performance.
本文描述了一种基于分子印迹聚合物(MIP)的新型选择性固相萃取方法。少量的 MIP 已在商业聚乙烯(PE)烧结体的孔内合成,并使用苯甲酮(BP)附着在其表面,BP 是一种能够从支撑材料表面引发聚合的光引发剂。优化了影响获得合适聚合层的关键性质,如聚合时间和交联剂种类。所开发的印迹材料已作为一种选择性吸附剂,用于从柑橘样品中提取噻菌灵(TBZ)作为模型化合物的提取物。研究了不同溶剂用于在印迹烧结体上加载分析物的情况,以及印迹聚合物的结合能力。当使用甲苯加载分析物时,印迹烧结体显示出良好的选择性,并且对于目标分析物,在 1000ng 加载分析物的范围内,获得了线性关系。制备的复合材料已应用于实际样品提取物中 TBZ 的 SPE,表现出令人印象深刻的净化能力。校准在原始固体样品浓度为 0.05-5.00μg g(-1)的范围内显示出良好的线性关系,所获得的回归系数大于 0.996。计算出的检测限为 0.016μg g(-1),足以满足对实际样品中 TBZ 的满意分析。在所有情况下,不同加标水平的 RSD 均低于 15%,并且印迹烧结体在不损失其性能的情况下可重复使用。