食品科学 ›› 2019, Vol. 40 ›› Issue (2): 310-317.doi: 10.7506/spkx1002-6630-20171020-216

• 安全检测 • 上一篇    下一篇

磁性分子印迹聚合物提取-超高效液相色谱-串联质谱法测定乳及乳制品中的4 种伪蛋白

单艺1,2,王象欣1,2,陈美君1,姜毓君1,2,3,满朝新1,2,3,马微4,*   

  1. (1.东北农业大学黑龙江省绿色食品科学研究院,黑龙江?哈尔滨 150028;2.东北农业大学食品学院,乳品科学教育部重点实验室,黑龙江?哈尔滨 150030;3.食品安全和营养协同创新中心,黑龙江?哈尔滨 150028;4.东宁出入境检验检疫局,黑龙江?东宁 157200)
  • 出版日期:2019-01-25 发布日期:2019-01-22
  • 基金资助:
    国家质检总局科技计划项目(2013IK155)

Determination of 4 Pseudo Proteins in Milk and Dairy Products by Magnetic Molecularly Imprinted Polymer Extraction-Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

SHAN Yi1,2, WANG Xiangxin1,2, CHEN Meijun1, JIANG Yujun1,2,3, MAN Chaoxin1,2,3, MA Wei4,*   

  1. (1. Heilongjiang Green Food Science Research Institute, Northeast Agricultural University, Harbin 150028, China;2. Key Lab of Dairy Science, Ministry of Education, School of Food Science, Northeast Agricultural University, Harbin 150030, China;3. Synergetic Innovation Center of Food Safety and Nutrition, Harbin 150028, China;4. Dongning Entry-Exit Inspection and Quarantine Bureau, Dongning 157200, China)
  • Online:2019-01-25 Published:2019-01-22

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-13C2和环丙氨嗪-D4为印记分子,Fe3O4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、0.50?μg/kg,在奶粉样品中的检出限分别为0.25、0.05、0.13、1.25?μg/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。

关键词: 磁性分子印迹聚合物, 伪蛋白, 超高效液相色谱-串联质谱

Abstract: 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-13C2 and cyromazine-D4 as templates and Fe3O4 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.

Key words: magnetic molecularly imprinted polymers, pseudo protein, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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