Hu Mei, Zhang Yijun, Yang Jinghua, Zhou Xiaomao, Wei Zhuqing, Ding Xiaoqing, Zhang Yuping
Se Pu. 2015 Feb;33(2):123-31. doi: 10.3724/sp.j.1123.2014.10008.
The rapid preparation of molecularly imprinted polymer (MIP) fibers was reported using bisphenol A (BPA) as the template molecular, acetonitrile (ACN) as the porogenic solvent, α-methacrylic acid (MAA) as the functional monomer, ethylene dimethacrylate (EDMA) as the crosslinker, and azodiisobutyronitrile (AIBN) as the thermal initiator. It was carried out within a capillary of 530 µm inner diameter (I. D.) by microwave irradiation in 7 min. The resulted BPA-MIP fibers were pushed out from the capillary, eluted in a vial and inserted in the capillary again followed by the application of the solid phase microextraction (SPME) procedure. The extraction performance was investigated in detail by varying the molar ratios between the template and the monomer (BPA/MAA), the concentration of NaCl, the extraction and desorption time, the pH value and the desorption solvents. The selectivity of the prepared MIP and non-molecularly imprinted polymer (NIP) fibers was comparatively evaluated by selecting two structurally-related compounds, phenol (P) and 4-phenylphenol (PP), and non-analogue dicyandiamide (DCD). The established method was successfully applied for the pretreatment and determination of BPA from beverage samples coupled to high performance liquid chromatography (HPLC). Under the optimal conditions, the linear range of BPA was 10-400 µg/L; the detection limit (LOD) was 0.45 µg/L and the recoveries spiked in the mineral water were 88.4%-102. 8%. The results demonstrated that the developed method can determine BPA in real samples with some advantages of simple pretreatment, rapid analysis, low limit of detection and low consumption of materials.
报道了以双酚A（BPA）为模板分子、乙腈（ACN）为致孔溶剂、α-甲基丙烯酸（MAA）为功能单体、乙二醇二甲基丙烯酸酯（EDMA）为交联剂、偶氮二异丁腈（AIBN）为热引发剂，快速制备分子印迹聚合物（MIP）纤维的方法。该过程在内径为530 µm的毛细管中通过微波辐射7分钟完成。将得到的BPA-MIP纤维从毛细管中推出，在小瓶中洗脱，然后再次插入毛细管，接着应用固相微萃取（SPME）程序。通过改变模板与单体之间的摩尔比（BPA/MAA）、NaCl浓度、萃取和解吸时间、pH值以及解吸溶剂，详细研究了萃取性能。通过选择两种结构相关的化合物苯酚（P）和4-苯基苯酚（PP）以及非类似物双氰胺（DCD），对制备的MIP纤维和非分子印迹聚合物（NIP）纤维的选择性进行了比较评估。所建立的方法成功应用于饮料样品中BPA的预处理和高效液相色谱（HPLC）测定。在最佳条件下，BPA的线性范围为10 - 400 µg/L；检测限（LOD）为0.45 µg/L，在矿泉水中加标的回收率为88.4% - 102.8%。结果表明，所开发的方法能够测定实际样品中的BPA，具有预处理简单、分析快速、检测限低和材料消耗少等优点。
