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基于可逆加成-断裂链转移聚合的磁性印迹聚合物对生物样品中卡马西平的选择性识别和富集。

Selective recognition and enrichment of carbamazepine in biological samples by magnetic imprinted polymer based on reversible addition-fragmentation chain transfer polymerization.

机构信息

Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, 211198, China.

Vocational and Technical College of Guizhou Minzu University, Guiyang, Guizhou, 550025, China.

出版信息

J Chromatogr A. 2019 Apr 26;1591:62-70. doi: 10.1016/j.chroma.2019.01.057. Epub 2019 Jan 26.

Abstract

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.

摘要

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。

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