Dipartimento di Scienza e Tecnologia del Farmaco, Torino, Italy.
J Sep Sci. 2010 Jun;33(11):1644-51. doi: 10.1002/jssc.201000013.
A cross-linked methacrylate molecularly imprinted polymer (poly-4-vinylpyridine-co-trimethylolpropane-trimethacrylate) selective for bisphenol A (BPA) was synthesized, using a fluorinated BPA derivative (4,4'-(hexafluoroisopropylidene)-diphenol) as a mimic template, and applied to the analysis of real-world samples of process and potable waters. The molecularly imprinted polymer also showed a high affinity and selectivity for 17-beta-estradiol and ethynylestradiol. A method to analyze BPA, 17-beta-estradiol, and ethynylestradiol at ultratrace levels was thus developed from a screening procedure to monitor endocrine-disrupting chemicals in water samples. The method consists of the BPA-selective cleanup by molecularly imprinted SPE using cartridges packed with the polymer developed, its recovery by stir bar sorptive extraction after ad hoc derivatization to obtain the corresponding BPA-acetate, and its analysis by GC-time window-SIM-MS after online thermal desorption. The method showed good linearity in the working range (R(2)=0.9969), high repeatability (RSD% <10.1), recoveries always above 90%, and very low LOD (10 pg/L) and LOQ (1 ng/L) and can easily be extended to the determination of 17-beta-estradiol and ethynylestradiol ultratraces. The method's effectiveness was evaluated by analyzing the real-world water samples; it enabled preconcentration and detection of BPA at ultratrace levels.
一种交联的甲基丙烯酸酯分子印迹聚合物(聚 4-乙烯基吡啶-co-三羟甲基丙烷-三甲基丙烯酸酯)被合成,以氟化双酚 A 衍生物(4,4' - (六氟异丙基)-二苯酚)为模拟模板,并应用于过程和饮用水实际样品的分析。该分子印迹聚合物对 17-β-雌二醇和乙炔雌二醇也表现出高亲和力和选择性。因此,从筛选程序中开发出了一种分析痕量 BPA、17-β-雌二醇和乙炔雌二醇的方法,以监测水样中的内分泌干扰化学物质。该方法包括使用装有开发的聚合物的分子印迹固相萃取进行 BPA 选择性净化,通过搅拌棒吸附萃取(SBSE)在特定衍生化后回收,以及在线热解吸后的 GC-时间窗口-SIM-MS 分析。该方法在工作范围内具有良好的线性(R(2)=0.9969),高重复性(RSD%<10.1),回收率始终高于 90%,并且具有非常低的检出限(10 pg/L)和定量限(1 ng/L),并且可以轻松扩展到痕量 17-β-雌二醇和乙炔雌二醇的测定。通过分析实际水样评估了该方法的有效性;它能够在痕量水平下进行 BPA 的预浓缩和检测。