College of Engineering, China Pharmaceutical University, No. 24 Tongjia Alley, Nanjing, PR China.
School of Science, China Pharmaceutical University, No. 24 Tongjia Alley, Nanjing, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2020 May 15;1145:122101. doi: 10.1016/j.jchromb.2020.122101. Epub 2020 Apr 6.
A highly efficient and selective method was successfully developed by using magnetic molecularly imprinted polymers (MMIPs) combined with high performance liquid chromatography (HPLC) to quickly determine patulin (PAT) in juice. MMIPs was prepared by surface imprinting method using FeO nanoparticles as supporter, 2-oxindole as virtual template, (3-Aminopropyl) triethoxysilane (APTES) as functional monomer and tetraethyl orthosilicate (TEOS) as crosslinking agent. The structure of the product was characterized by vibrating sample magnetometer (VSM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). The results showed that MMIP with a particle size of about 450 nm was successfully prepared, the imprinted molecular layer accounted for about 11.6% of the total mass, and the saturation magnetization was about 6.82 emu/g. The maximum adsorption capacities (Qmax) of kinetic and thermodynamic adsorption experiments were 1.97 mg/g and 4.241 mg/g, respectively. The adsorption process was highly selective and fitted well with the pseudo-second-order model. Langmuir model demonstrated that the binding sites were evenly distributed on the surface of the MMIPs. Scatchard analysis showed that MMIPs had two types of binding sites with Qmax of 4.53 mg/g and 5.73 mg/g, respectively. In the actual sample application, the limit of detection (LOD) and the limit of quantification (LOQ) were 3 μg/kg and 10 μg/kg. And the recovery rate of the sample was 86.44-95.50%. MMIPs possessed excellent applicability with stability of 1.11-3.16% and accuracy of 0.63-1.94%. These results indicated that MMIPs had good performance in separating PAT and was suitable for determining PAT in actual samples.
采用磁性分子印迹聚合物（MMIPs）结合高效液相色谱（HPLC）成功开发了一种快速测定果汁中棒曲霉素（PAT）的高效、选择性方法。以 FeO 纳米粒子为载体，以 2-氧吲哚为虚拟模板，（3-氨丙基）三乙氧基硅烷（APTES）为功能单体，正硅酸乙酯（TEOS）为交联剂，采用表面印迹法制备 MMIPs。采用振动样品磁强计（VSM）、傅里叶变换红外光谱（FT-IR）、X 射线衍射（XRD）和热重分析（TGA）对产物的结构进行了表征。结果表明，成功制备了粒径约为 450nm 的 MMIP，印迹分子层占总质量的约 11.6%，饱和磁化强度约为 6.82emu/g。动力学和热力学吸附实验的最大吸附容量（Qmax）分别为 1.97mg/g 和 4.241mg/g。吸附过程具有高度选择性，与拟二级动力学模型拟合良好。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，其 Qmax 分别为 4.53mg/g 和 5.73mg/g。在实际样品应用中，检测限（LOD）和定量限（LOQ）分别为 3μg/kg 和 10μg/kg。样品的回收率为 86.44%-95.50%。MMIPs 具有良好的适用性，稳定性为 1.11%-3.16%，准确度为 0.63%-1.94%。这些结果表明，MMIPs 在分离 PAT 方面具有良好的性能，适用于测定实际样品中的 PAT。
