Yan Hongyuan, Row Kyung Ho
Center for Advanced Bioseparation Technology, Department of Chemical Engineering, Inha University, Incheon, 402-751, Korea.
Biomed Chromatogr. 2008 May;22(5):487-93. doi: 10.1002/bmc.957.
Water-compatible ciprofloxacin-imprinted monolithic columns were synthesized in water-containing systems for selective extraction of ciprofloxacin from human urine samples. Methanol-water (10:3, v/v) was used as a porogenic solvent and the obtained monolithic imprinted polymers reveal high selectivity to ciprofloxacin in an aqueous environment; the affinity can be easily controlled by adjusting the pH of the mobile phase. Owing to the unique porous structure and flow-through channels existing in the network skeleton of the monolithic MIP, urine samples could be directly injected into the column, proteins and other biological matrix were quickly washed out and ciprofloxacin was selectively retained and enriched. Good linearity was obtained from 0.08 to 400 mg/L (r=0.998) with the relative standard deviations less than 3.6%. The limit of detection of the method was 0.04 mg/L and the recoveries were more than 94.5% at three different concentrations. Moreover, by increasing the injection volume to 2.0 mL, the sensitivity of the method could be improved 100-fold according to the peak height of ciprofloxacin. This expedient greatly simplified the overall procedure, resulting in a rapid and efficient sample analysis while maintaining precision and accuracy.
在含水体系中合成了与水相容的环丙沙星印迹整体柱,用于从人尿液样本中选择性萃取环丙沙星。以甲醇 - 水(10:3,v/v)作为致孔剂,所制备的整体印迹聚合物在水环境中对环丙沙星表现出高选择性;通过调节流动相的pH值可轻松控制其亲和力。由于整体分子印迹聚合物网络骨架中存在独特的多孔结构和贯穿通道,尿液样本可直接进样到柱中,蛋白质和其他生物基质能被快速洗脱,而环丙沙星被选择性保留和富集。在0.08至400 mg/L范围内获得了良好的线性关系(r = 0.998),相对标准偏差小于3.6%。该方法的检测限为0.04 mg/L,在三个不同浓度下回收率均超过94.5%。此外,通过将进样体积增加到2.0 mL,根据环丙沙星的峰高,该方法的灵敏度可提高100倍。此方法极大地简化了整个流程,在保持精密度和准确度的同时实现了快速高效的样品分析。