应用化学

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三聚氰胺磁性印迹固相萃取材料的制备及其应用

刘玉楠1,2,张朝晖1,2,3*,陈星1,陈红军1,饶维1,蔡蓉1   

  1. (1.吉首大学林产化工重点实验室 张家界 427000;2.吉首大学化学化工学院 吉首 416000;
    3.湖南大学化学生物传感与计量国家重点实验室 长沙 410082)
  • 收稿日期:2013-01-08 修回日期:2013-03-11 出版日期:2013-10-10 发布日期:2013-10-10
  • 通讯作者: 张朝晖,副教授; Tel/Fax:0743-8563911; E-mail:zhaohuizhang77@163.com; 研究方向:印迹色谱分析和电化学分析
  • 基金资助:
    国家自然科学基金(21005030和21267010)和湖南省高校科技创新团队资助

Preparation and Application of Melamine Magnetic Molecularly Imprinted Solid Phase Extraction Material

LIU Yunan1,2, ZHANG Zhaohui1,2,3*, CHEN Xing1, CHEN Hongjun1, RAO Wei1, CAI Rong1   

  1. (1.Key Laboratory of Hunan Forest Products and Chemical Industry Engineering,
    Jishou University,Zhangjiajie 427000,China;
    2.College of Chemistry and Chemical Engineering,Jishou University,Jishou 416000,China;
    3.State Key Laboratory of Chemo/Biosensing and Chemometrics,Hunan University,Changsha 410082,China)
  • Received:2013-01-08 Revised:2013-03-11 Published:2013-10-10 Online:2013-10-10

摘要: 采用磁性氧化石墨烯(GO)为载体,三聚氰胺(MEL)为模板分子,甲基丙烯酸(MAA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)为交联剂,制备了新型三聚氰胺磁性印迹聚合物。 采用扫描电子显微镜(SEM)、透射电子显微(TEM)、差热分析(TG)和样品振动磁强计(VSM)对该磁性印迹聚合物进行表征和分析,结果表明,在氧化石墨烯表面成功制备磁性印迹聚合物。 结合高效液相色谱分析技术对该印迹聚合物的吸附性能进行检测,结果表明,该磁性印迹聚合物对三聚氰胺表现出特异性吸附性能,最大吸附容量为33.11 mg/g;相对于环丙氨嗪和三聚氰酸,三聚氰胺的选择因子(β)分别是2.43和2.84。 结合磁固相萃取与液相色谱检测技术,实现了牛奶样品溶液中三聚氰胺的分离、富集和检测。

关键词: 印迹聚合物, 三聚氰胺, 磁性氧化石墨烯, 磁固相萃取技术, 高效液相色谱

Abstract: A novel melamine magnetic molecularly imprinted polymer(Fe3O4-GO@SiO2@MIP) was prepared based on graphene oxide(GO) using melamine(MEL) as the template molecule, methacrylic acid(MAA) as the functional monomer and ethylene glycol dimethacrylate(EGDMA) as the cross-linker. The Fe3O4-GO@SiO2@MIP was characterized by scanning electron microscope(SEM), transmission electron microscope(TEM), thermogravimetric analysis(TGA) and vibrating sample magnetometer(VSM). The results showed that MEL imprinted layer was grafted on magnetic GO surface successfully. The adsorption properties were investigated by high performance liquid chromatography, and the results demonstrated that the Fe3O4-GO@SiO2@MIP exhibited specific selectivity towards MEL. The maximum adsorption capacity of Fe3O4-GO@SiO2@MIP is 33.11 mg/g, and the selectivity factor of MEL towards CYR and CYA is 2.43 and 2.84, respectively. Combined with magnetic solid phase extraction(M-SPE) and high-performance liquid chromatography with the imprinted material as stationary phase, melamine from the sample solution of milk was successfully separated, enriched and detected.

Key words: Imprinted polymer, Melamine, Magnetic graphene oxide, Magnetic solid phase extraction, High-performance liquid chromatography

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