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Synthesis of metronidazole-imprinted molecularly imprinted polymers by distillation precipitation polymerization and their use as a solid-phase adsorbent and chromatographic filler

机译:蒸馏沉淀聚合法合成甲硝唑印迹分子印迹聚合物及其作为固相吸附剂和色谱填料的用途

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摘要

Metronidazole-imprinted polymers with superior recognition properties were prepared by a novel strategy called distillation-precipitation polymerization. The as-obtained polymers were characterized by Fourier-transform infrared spectroscopy, laser particle size determination and scanning electron microscopy, and their binding performances were evaluated in detail by static, kinetic and dynamic rebinding tests, and Scatchard analysis. The results showed that when the fraction of the monomers was 5 vol% in the whole reaction system, the prepared polymers afforded good morphology, monodispersity, and high adsorption capacity and excellent selectivity to the target molecule, metronidazole. The optimal binding performance is 12.41 mg/g for metronidazole just before leakage occurred and 38.51 mg/g at saturation in dynamic rebinding tests. Metronidazole-imprinted polymers were further applied as packing agents in solid-phase extraction and as chromatographic filler, both of which served for the detection of metronidazole in fish tissue. The results illustrated the recoveries of spiked samples ranged from 82.97 to 87.83% by using molecularly imprinted solid-phase extraction combined with a C-18 commercial column and 93.7 to 101.2% by directly using the polymer-packed chromatographic column. The relative standard deviation of both methods was less than 6%.
机译:具有卓越识别性能的甲硝唑印迹聚合物是通过一种称为蒸馏-沉淀聚合的新策略制备的。通过傅立叶变换红外光谱,激光粒度测定和扫描电子显微镜对所获得的聚合物进行表征,并通过静态,动力学和动态再结合测试以及Scatchard分析来详细评估其结合性能。结果表明,当在整个反应体系中单体的含量为5vol%时,所制备的聚合物具有良好的形态,单分散性,高吸附容量和对目标分子甲硝唑的优异选择性。在动态重新结合试验中,甲硝唑的最佳结合性能是在发生泄漏之前对甲硝唑为12.41 mg / g,在饱和时为38.51 mg / g。甲硝唑印迹聚合物进一步用作固相萃取中的包装剂和色谱填充剂,两者均用于检测鱼组织中的甲硝唑。结果表明,使用分子印迹固相萃取结合C-18商业色谱柱,加标样品的回收率在82.97%至87.83%之间,而直接使用聚合物填充色谱柱的回收率在93.7%至101.2%之间。两种方法的相对标准偏差均小于6%。

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