Behbahani Mohammad, Bagheri Saman, Amini Mostafa M, Sadeghi Abandansari Hamid, Reza Moazami Hamid, Bagheri Akbar
Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran, Iran.
J Sep Sci. 2014 Jul;37(13):1610-6. doi: 10.1002/jssc.201400188. Epub 2014 May 2.
Magnetic molecularly imprinted polymers have been synthesized for the selective preconcentration and trace determination of lamotrigine (LTG) in urine and plasma samples. The magnetic nanoparticles were modified by tetraethyl orthosilicate and 3-methacryloxypropyl trimethoxysilane before imprinting. The magnetic molecularly imprinted polymers were prepared via surface molecular imprinting technique, using Fe3 O4 as a magnetic component, LTG as template molecule, methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, and 2,2'-azobisisobutyronitrile as a radical initiator in methanol/acetonitrile (50:50, v/v) as the porogen. The obtained sorbent was characterized using scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, and thermal analysis. Separation of the sorbent from the sample solution was simply achieved by applying an external magnetic field. Determination of the extracted drug was performed by high-performance liquid chromatography with UV detection. Under the optimum extraction conditions, the method detection limits were 0.7 μg/L (based on S/N of 3) for urine samples and 0.5 μg/L for plasma samples. A linear dynamic range of 1-1000 μg/L was obtained for LTF in plasma and urine samples. Finally, the applicability of the proposed method was evaluated by extraction and determination of LTG in urine and plasma samples.
已合成磁性分子印迹聚合物,用于尿液和血浆样品中拉莫三嗪(LTG)的选择性预富集和痕量测定。在印迹之前,用正硅酸四乙酯和3-甲基丙烯酰氧基丙基三甲氧基硅烷对磁性纳米颗粒进行改性。以Fe3O4为磁性成分,LTG为模板分子,甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,2,2'-偶氮二异丁腈为自由基引发剂,在甲醇/乙腈(50:⁵⁰,v/v)作为致孔剂的条件下,通过表面分子印迹技术制备磁性分子印迹聚合物。使用扫描电子显微镜、傅里叶变换红外光谱、X射线衍射和热分析对所得吸附剂进行表征。通过施加外部磁场可简单地实现吸附剂与样品溶液的分离。采用高效液相色谱-紫外检测法对提取的药物进行测定。在最佳提取条件下,该方法对尿液样品的检测限为0.7μg/L(基于3的信噪比),对血浆样品的检测限为0.5μg/L。血浆和尿液样品中LTF的线性动态范围为1-1000μg/L。最后,通过对尿液和血浆样品中LTG的提取和测定,评估了该方法的适用性。