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Core-shell nano-sized magnetic molecularly imprinted solid phase extractant coupled with HPLC for the selective isolation and determination of 17 beta-estradiol in a lake water sample

机译:核-壳纳米级磁性分子印迹固相萃取剂与HPLC结合用于湖水中样品中17β-雌二醇的选择性分离和测定

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摘要

In this work, a novel type of core-shell molecularly imprinted magnetic nanoparticles was synthesized and coupled with HPLC for the selective extraction and detection of 17 beta-estradiol (E2) in lake water samples. The synthesis procedure combined a surface imprinting technique and a facile sol-gel strategy. The morphology, structure, and magnetic properties of the obtained products were characterized by transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and vibrating sample magnetometer. The adsorption properties of the prepared polymers were investigated by equilibrium rebinding, dynamic adsorption, and selective recognition experiments. The resultant imprinted nanomaterials exhibit not only good dispersibility, stable crystalline structure, and satisfactory super-paramagnetic properties, but also fast kinetics, high capacity (16.87 mg g(-1)), and favorable selectivity. In addition, the as-synthesized polymers show good reproducibility and could be used for at least six cycles of adsorption-desorption without obvious deterioration. The feasibility of the developed method using the obtained imprinted polymers as a SPE extractant coupled with HPLC for the selective isolation and determination of E2 from real water samples was demonstrated. The recovery of E2 in a lake water sample ranged from 94.2 to 98.3% with the relative standard deviation less than 4.3%. The combined method would greatly improve the sensitivity and expand the practicability of HPLC.
机译:在这项工作中,合成了一种新型的核-壳分子印迹磁性纳米颗粒,并与HPLC结合用于选择性提取和检测湖水样品中的17β-雌二醇(E2)。合成过程结合了表面压印技术和简便的溶胶-凝胶策略。通过透射电子显微镜,X射线衍射,傅立叶变换红外光谱和振动样品磁强计对所得产物的形貌,结构和磁性进行了表征。通过平衡结合,动态吸附和选择性识别实验研究了所制备聚合物的吸附性能。所得的印迹纳米材料不仅显示出良好的分散性,稳定的晶体结构和令人满意的超顺磁性能,而且还显示出快速的动力学,高容量(16.87 mg g(-1))和良好的选择性。另外,所合成的聚合物显示出良好的可再现性,并且可以用于至少六个吸附-解吸循环而没有明显的劣化。证明了使用所获得的印迹聚合物作为SPE萃取剂和HPLC进行开发的方法从实际水样中选择性分离和测定E2的可行性。湖泊水样中E2的回收率介于94.2%至98.3%之间,相对标准偏差小于4.3%。结合的方法将大大提高灵敏度,并扩大HPLC的实用性。

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