摘要
建立磁性分子印迹聚合物(magnetic molecular imprinted polymers,MMIPs)提取结合超高效液相色谱-串联质谱法测定乳及乳制品中4种伪蛋白(三聚氰胺、环丙氨嗪、双氰胺和缩二脲)的方法。以缩二脲-~(13)C_2和环丙氨嗪-D_4为印记分子,Fe_3O_4为磁性组分,制备具有特异识别性的MMIPs提取样品中的目标化合物,超高效液相色谱-串联质谱法检测。结果表明,4种化合物在5~200 ng/mL范围内具有良好的线性关系,线性相关系数大于0.999。三聚氰胺、环丙氨嗪、双氰胺和缩二脲在牛奶样品中的检出限分别为0.10、0.02、0.05、0.50μg/kg,在奶粉样品中的检出限分别为0.25、0.05、0.13、1.25μg/kg。回收率为80.5%~96.1%,相对标准偏差为1.1%~9.2%。利用本方法对实际样品中4种化合物进行测定,分析结果显示该方法所得到的数值准确、可靠。
A simple and rapid method for the determination of 4 pseudo proteins including melamine, cyromazine, dicyandiamide and biuret in milk and dairy products has been developed by using magnetic molecularly imprinted polymers (MMIPs) extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The MMIPs used for the extraction of 4 pseudo proteins were synthesized by polymerization using biuret-~(13)C_2 and cyromazine-D_4 as templates and Fe_3O_4 magnetite as magnetic component. Under the optimized conditions, good linearity was observed for all target analytes in the concentration range of 5–200 ng/mL with correlation coefficient above 0.999. The limits of detection (LODs) for melamine, cyromazine, dicyandiamide and biure were 0.10, 0.02, 0.05 and 0.50 μg/kg in milk samples and 0.25, 0.05, 0.13 and 1.25 μg/kg in powered milk samples, respectively. The recoveries were between 80.5%and 96.1% with relative standard deviations (RSDs) between 1.1% and 9.2%. The developed method was applied with good precision and accuracy to determine real dairy samples.
引文
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