Zhao Xiaoyu, Chen Ligang
Department of Chemistry, College of Science, Northeast Forestry University, China.
J Sep Sci. 2016 Oct;39(19):3775-3781. doi: 10.1002/jssc.201600625. Epub 2016 Sep 6.
A new magnetic molecularly imprinted polymer was coupled with ultra high performance liquid chromatography and tandem mass spectrometry for the selective determination of melamine in milk powder. The magnetic molecularly imprinted polymer has been prepared by using carbon nanotubes as the matrix, Fe O particles as the magnetic ingredient, melamine as the template molecule, methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker and polyvinylpyrrolidone as the dispersant. The polymer was characterized with scanning electron microscopy, Fourier transform infrared spectroscopy and a physical property measurement system. The isothermal adsorption, kinetics adsorption, and selectivity were studied to evaluate the rebinding properties of the magnetic molecularly imprinted polymer. Various parameters affecting the extraction efficiency such as the amount of polymer, extraction time, and eluting solution were evaluated. The limit of detection was 0.00075 mg/kg. The relative standard deviations of the intraday and interday precision are 0.4-2.7 and 2.3-5.1%, respectively. The proposed method was successfully applied to determine melamine in different milk powder samples from different provenances, and satisfactory recoveries of 89.0-95.6% were obtained. This method has great significance for quality control and is simple and suitable for the rapid determination of melamine in milk powder.
一种新型磁性分子印迹聚合物与超高效液相色谱-串联质谱联用,用于选择性测定奶粉中的三聚氰胺。该磁性分子印迹聚合物以碳纳米管为基质、Fe₃O₄颗粒为磁性成分、三聚氰胺为模板分子、甲基丙烯酸为功能单体、乙二醇二甲基丙烯酸酯为交联剂、聚乙烯吡咯烷酮为分散剂制备而成。采用扫描电子显微镜、傅里叶变换红外光谱和物理性能测量系统对该聚合物进行了表征。研究了等温吸附、动力学吸附和选择性,以评估磁性分子印迹聚合物的再结合性能。评估了聚合物用量、萃取时间和洗脱液等影响萃取效率的各种参数。检测限为0.00075 mg/kg。日内精密度和日间精密度的相对标准偏差分别为0.4 - 2.7%和2.3 - 5.1%。该方法成功应用于测定不同产地的不同奶粉样品中的三聚氰胺,回收率为89.0 - 95.6%,结果令人满意。该方法对质量控制具有重要意义,且操作简单,适用于奶粉中三聚氰胺的快速测定。