食品科学 ›› 2017, Vol. 38 ›› Issue (20): 203-208.doi: 10.7506/spkx1002-6630-201720029

• 安全检测 • 上一篇    下一篇

分子印迹固相萃取-高效液相色谱法检测奶粉中的双氰胺

刘慧琳,倪天鸿,周凯文,王静   

  1. (北京食品营养与人类健康高精尖创新中心,北京市食品添加剂工程技术研究中心,北京工商大学,北京 100048)
  • 出版日期:2017-10-25 发布日期:2017-09-29
  • 基金资助:
    国家自然科学基金青年科学基金项目(31501559);国家自然科学基金面上项目(31571940); 北京市教委一般项目(201610011004)

Molecularly Imprinted Solid-Phase Extraction Coupled with High Performance Liquid Chromatography for the Detection of Dicyandiamide in Milk Powder

LIU Huilin, NI Tianhong, ZHOU Kaiwen, WANG Jing   

  1. (Beijing Advanced Innovation Center for Food Nutrition and Human Health, Beijing Engineering and Technology Research Center of Food Additives, Beijing Technology & Business University (BTBU), Beijing 100048, China)
  • Online:2017-10-25 Published:2017-09-29

摘要: 通过一步聚合法制备以双氰胺为模板分子,甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸为交联剂,偶氮二异丁腈为引发剂的分子印迹聚合物。通过扫描电子显微镜、红外光谱、紫外光谱等对材料的物理及化学性能进行表征。采用分子印迹固相萃取结合高效液相色谱法检测实际奶粉样品中的双氰胺残留。该方法的线性范围为0.01~2.00?mg/L,线性相关系数R2为0.999?4,呈现良好的线性关系,检出限(RSN=3)为0.57×10-2?mg/L,样品加标回收率为102.5%~104%,相对标准偏差在0.21%~0.86%之间。

关键词: 双氰胺, 分子印迹聚合物, 固相萃取, 高效液相色谱

Abstract: A novel molecularly imprinted polymer was developed by a one-step polymerization using dicyandiamide as template, methacrylic acid as functional monomer, ethylene glycol dimethylacrylate as cross-linker, and azobisisobutyronitrile as initiator. The physicochemical properties of the prepared material were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and ultraviolet spectroscopy. A molecularly imprinted solid phase extraction coupled with high performance liquid chromatography method was developed using this material to detect dicyandiamide in real milk powder samples. The linear range of this method was from 0.01 to 2.00 mg/L, with a correlation coefficient (R2) equal to 0.999 4, which had a good linear relationship. The limit of detection (LOD) was 0.57 × 10-2 mg/L (RSN = 3). The recovery was ranged from 102.5% to 104%, and the relative standard deviation was between 0.21% and 0.86%.

Key words: dicyandiamide, molecularly imprinted polymers (MIP), solid-phase extraction, high performance liquid chromatography (HPLC)

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