Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, 211198, China.
Vocational and Technical College of Guizhou Minzu University, Guiyang, Guizhou, 550025, China.
J Chromatogr A. 2019 Apr 26;1591:62-70. doi: 10.1016/j.chroma.2019.01.057. Epub 2019 Jan 26.
A well-defined molecularly imprinted polymer (FeO@CS@MIP) was synthesized via reversible addition-fragmentation chain transfer polymerization for magnetic solid-phase extraction coupled with high-performance liquid chromatography-diode array detector to detect carbamazepine (CBZ) in biological samples. The composition of FeO@CS@MIP was selected by a two-step screening method. 4-vinyl pyridine, divinylbenzene and dimethylformamide were chosen as the functional monomer, cross-linker and porogen, respectively. The imprinted layer was coated on the surface of the chain transfer agent-modified magnetic chitosan nanoparticles. The prepared FeO@CS@MIP was characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller measurement and vibrating sample magnetometer. The results indicated that FeO@CS@MIP had a large surface area (265.8 m/g), high saturation magnetization (19.88 emu/g) and uniform structure. Besides, the binding property of the FeO@CS@MIP was studied in detail. The FeO@CS@MIP showed high imprinting factor (IF = 4.83) and desirable adsorption capacity (323.10 μmol/g) to CBZ. Under the optimum conditions, the developed method exhibited excellent linearity (R>0.999) in the range of 0.01-0.5 mg/L and 1.0-30.0 mg/L, and the limits of detection were 1.0 μg/L and 9.6 μg/L for the urine and serum samples, respectively. Good recoveries (88.22%-101.18%) were obtained with relative standard deviations less than 4.83%. This work provided a practical approach for the selective extraction and detection of CBZ in real samples.
通过可逆加成-断裂链转移聚合，合成了一种具有明确分子印迹的聚合物（FeO@CS@MIP），用于磁性固相萃取结合高效液相色谱-二极管阵列检测，以检测生物样品中的卡马西平（CBZ）。通过两步筛选法选择 FeO@CS@MIP 的组成。4-乙烯基吡啶、二乙烯基苯和二甲基甲酰胺分别选为功能单体、交联剂和致孔剂。印迹层涂覆在链转移剂修饰的磁性壳聚糖纳米粒子表面。通过扫描电子显微镜、透射电子显微镜、傅里叶变换红外光谱、BET 测量和振动样品磁强计对 FeO@CS@MIP 进行了表征。结果表明，FeO@CS@MIP 具有较大的比表面积（265.8 m2/g）、高饱和磁化强度（19.88 emu/g）和均匀的结构。此外，还详细研究了 FeO@CS@MIP 的结合性能。FeO@CS@MIP 对 CBZ 表现出较高的印迹因子（IF=4.83）和理想的吸附容量（323.10 μmol/g）。在最佳条件下，该方法在 0.01-0.5 mg/L 和 1.0-30.0 mg/L 范围内表现出良好的线性（R>0.999），尿液和血清样品的检测限分别为 1.0 μg/L 和 9.6 μg/L。回收率良好（88.22%-101.18%），相对标准偏差小于 4.83%。这项工作为实际样品中 CBZ 的选择性提取和检测提供了一种实用方法。
