College of Engineering, China Pharmaceutical University, No. 24 Tongjia Alley, Nanjing, 210009, Jiangsu, China.
School of Science, China Pharmaceutical University, No. 24 Tongjia Alley, Nanjing, 210009, Jiangsu, China.
Anal Bioanal Chem. 2020 Jul;412(19):4725-4737. doi: 10.1007/s00216-020-02729-y. Epub 2020 May 31.
This study was based on the specific binding ability of magnetic molecularly imprinted polymers (MMIPs) combined with a high-performance liquid chromatography-fluorescence detector (HPLC-FLD) for the rapid determination of zearalenone (ZEN) in cereals. A novel magnetic molecularly imprinted polymer was prepared by surface imprinting technology. Warfarin was used as a virtual template, 3-aminopropyl triethoxysilane (APTES) was used as the functional monomer, and tetraethyl orthosilicate (TEOS) was used as the cross-linking agent. Analysis by a vibrating sample magnetometer (VSM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) showed that MMIPs were prepared with a particle size about 450 nm, the imprinted molecular layer accounting for 10.7% of the total mass, and saturation magnetization of about 34.54 emu/g. The maximum adsorption capacity (Q) of the thermodynamic and kinetic adsorption experiments were 13.90 mg/g and 8.71 mg/g, respectively. The Langmuir model showed that the binding sites were uniformly distributed on the surface of the MMIPs. The Scatchard analysis showed that MMIPs had two types of binding sites with Q of 8.22 mg/g and 15.37 mg/g, respectively. In actual sample detection, the limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/kg and 0.9 ng/kg, respectively. The sample recovery rate was 90.56-99.96%, the daytime stability was 1.35-2.87%. These results showed that MMIPs had good performance in selectively identifying ZEN and were suitable for determining ZEN in cereals.
本研究基于磁性分子印迹聚合物(MMIPs)的特异性结合能力,结合高效液相色谱-荧光检测器(HPLC-FLD),用于快速测定谷物中的玉米赤霉烯酮(ZEN)。采用表面印迹技术制备了一种新型磁性分子印迹聚合物。华法林被用作虚拟模板,3-氨丙基三乙氧基硅烷(APTES)用作功能单体,正硅酸乙酯(TEOS)用作交联剂。通过振动样品磁强计(VSM)、傅里叶变换红外光谱(FT-IR)、X 射线衍射(XRD)、热重分析(TGA)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)分析表明,MMIPs 的粒径约为 450nm,印迹分子层占总质量的 10.7%,饱和磁化强度约为 34.54 emu/g。热力学和动力学吸附实验的最大吸附容量(Q)分别为 13.90mg/g 和 8.71mg/g。Langmuir 模型表明,结合位点均匀分布在 MMIPs 表面。Scatchard 分析表明,MMIPs 具有两种类型的结合位点,Q 值分别为 8.22mg/g 和 15.37mg/g。在实际样品检测中,检测限(LOD)和定量限(LOQ)分别为 0.4ng/kg 和 0.9ng/kg。样品回收率为 90.56-99.96%,日间稳定性为 1.35-2.87%。这些结果表明,MMIPs 对 ZEN 具有良好的选择性识别性能,适用于谷物中 ZEN 的测定。