Department of Analytical Chemistry, China Pharmaceutical University, 24 Tongjia Lane, Nanjing 210009, Jiangsu, China.
Analyst. 2013 Jun 7;138(11):3287-96. doi: 10.1039/c3an36755j.
Fluoroquinolones (FQs) have emerged as one of the most important class of antibiotics. Due to their low concentration in bio-matrix samples which contain a lot of interfering substances, the efficient solid phase extraction and accurate determination of FQs remain a challenge. In this paper, a new strategy for the isolation and enrichment of FQs from egg samples was obtained by molecularly imprinted polymers on the surface of magnetic carbon nanotubes (MCNTs@MIP), which not only can be collected and separated rapidly by an external magnetic field, but also have a high specific surface area, outstanding mechanical properties and specific recognition for FQs. MCNTs@MIP were prepared using ofloxacin as a pseudo template, methacrylic acid as a functional monomer, and ethylene glycol dimethacrylate as a cross-linker. The characteristics of the MCNTs@MIP were assessed by transmission electron microscopy (TEM), multipoint Brunauer-Emmett-Teller (BET) analysis, vibrating sample magnetometry (VSM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. The results of the adsorption experiments not only demonstrated rapid dynamic adsorption but also showed a high selectivity toward FQs. An extraction method using MCNTs@MIP coupled with high performance liquid chromatography (HPLC) was developed for the determination of four FQs in egg samples. The recovery of four FQs ranged from 95.2% ± 3.2% to 100.7% ± 3.1% and the detection limits ranged from 0.25-0.40 ng g(-1). The results demonstrate that the proposed method based on pseudo template MCNTs@MIP is a promising approach for the preconcentration, purification, and simultaneous analysis of four FQs in bio-matrix samples.
氟喹诺酮类(FQs)已成为最重要的抗生素类别之一。由于它们在含有大量干扰物质的生物基质样品中的浓度较低,因此高效的固相萃取和 FQs 的准确测定仍然是一个挑战。在本文中,通过在磁性碳纳米管(MCNTs@MIP)表面上的分子印迹聚合物获得了从鸡蛋样品中分离和富集 FQs 的新策略,其不仅可以通过外部磁场快速收集和分离,而且还具有高比表面积、出色的机械性能和对 FQs 的特异性识别。使用氧氟沙星作为伪模板、甲基丙烯酸作为功能单体和乙二醇二甲基丙烯酸酯作为交联剂制备 MCNTs@MIP。通过透射电子显微镜(TEM)、多点 Brunauer-Emmett-Teller(BET)分析、振动样品磁强计(VSM)、X 射线衍射(XRD)和傅里叶变换红外(FT-IR)光谱评估 MCNTs@MIP 的特性。吸附实验的结果不仅证明了快速动态吸附,而且还表现出对 FQs 的高选择性。开发了一种使用 MCNTs@MIP 与高效液相色谱(HPLC)结合的萃取方法,用于测定鸡蛋样品中的四种 FQs。四种 FQs 的回收率范围为 95.2%±3.2%至 100.7%±3.1%,检测限范围为 0.25-0.40ng g(-1)。结果表明,基于伪模板 MCNTs@MIP 的方法是一种很有前途的方法,可用于生物基质样品中四种 FQs 的预浓缩、纯化和同时分析。