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作 者:赵海青[1] 江梦银 冯莹莹[1] 吴安乐[1] 詹晓珠 邓健[1]
机构地区:[1]南华大学化学化工学院,湖南衡阳421001 [2]福建省三明市农产品质量安全检验中心,福建三明365000
出 处:《分析测试学报》2016年第8期993-998,共6页Journal of Instrumental Analysis
基 金:南华大学研究生科研创新项目(2015XCX16);湖南省科技厅项目(2013FJ3028)
摘 要:以罗硝唑(Ronidazole,RNZ)为模板,3-氨丙基三乙氧基硅烷为功能单体,Al(Ⅲ)为路易斯酸掺杂剂,用溶胶-凝胶法制备核壳型磁性分子印迹聚合物,借助磁力作用将其修饰于磁性玻碳电极表面,制得RNZ电化学印迹传感器。以透射电镜、红外光谱、X-射线衍射及电化学方法等对该传感器进行表征,并对影响传感器性能的主要参数进行优化。结果表明,相比基于非掺杂印迹聚合物和非分子印迹聚合物的传感器,铝掺杂印迹传感器对罗硝唑具有更强的结合能力和更高的识别选择性。用差分脉冲溶出伏安法进行定量测定时,RNZ的还原峰电流与其浓度在0.05~50.0μmol/L范围内呈良好线性关系(r=0.997 3),检出限为0.015μmol/L。对牛奶、鸡蛋中RNZ的回收率为88.6%~97.0%,相对标准偏差(RSD)为2.9%~4.6%。An electrochemical sensor for the determination of ronidazole (RNZ) was developed based on a magnetic glassy carbon electrode modified with AI(Ⅲ) doped core-shell magnetic surface molec- ularly imprinted polymer (MMIP), which was prepared via the sol-gel method using RNZ as tem- plate, 3-aminopropyhriethoxysilane as functional monomer, orthosilicate as cross-linker, and Al3+ as dopant to generate Lewis acid sites in the silica matrix for the metal coordinate interactions with the template RNZ. The component, morphology of MMIP and the performance of the as-prepared sensor were characterized by transmission electron microscopy, Fourier transform infrared spectroscopy, powder X-ray diffraction and the electrochemical methods. Various factors affecting the response be- havior of the sensor were studied and optimized. Because of the aluminum doping, the imprinted sensor exhibits the best recognition ability and affinity for RNZ in comparison with the aluminum free MMIP and the non-imprinted one. Under the optimal experimental conditions, the peak currents by differential pulse stripping voltammetry were found to vary linearly with RNZ concentrations in the range of 0.05 - 50. 0 μmol/L with a detection limit of 0. 015 μmol/L. This sensor was successfully employed to detect RNZ in milk powder and egg samples with recoveries of 88.6% - 97.0% and rela- tive standard deviations of 2.9% -4.6%.
关 键 词:罗硝唑 磁性表面分子印迹聚合物 差分脉冲溶出伏安法 铝掺杂
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