以改性松香为交联剂的甲硝唑磁性分子印迹固相萃取材料的制备、表征及分子识别性研究

doi:10.16333/j.1001-6880.2016.1.005

天然产物研究与开发 ›› 2016, Vol. 28 ›› Issue (1): 23-29.doi: 10.16333/j.1001-6880.2016.1.005

以改性松香为交联剂的甲硝唑磁性分子印迹固相萃取材料的制备、表征及分子识别性研究

刘敏，吴宗远，李小燕*，王芳，李鹏飞

广西民族大学化学化工学院广西高校食品安全与药物分析化学重点实验室广西林产化学与工程重点实验室广西高校微生物与植物资源利用重点实验室，南宁 530008

出版日期:2016-01-29 发布日期:2016-02-01

Synthesis,Characterization and Molecular Recognition Property of Magnetic Molecularly Imprinted Polymers Microspheres with Modified Rosin as Cross-linking agent for Solid Phase Extraction of Metronidazole

LIU Min,WU Zong-yuan,LI Xiao-yan*,WANG Fang,LI Peng-fei

School of Chemistry and Chemical Engineering,Guangxi University for Nationalities,Key Laboratory of Guangxi Colleges and Universities for Food Safety and Pharmaceutical Analytical Chemistry,Guangxi Key Laboratory of Chemistry and Engineering of Forest Products,Guangxi Colleges and Universities Key Laboratory of Utilization of Microbial and Botanical Resources,Nanning 530008,China

Online:2016-01-29 Published:2016-02-01

摘要/Abstract

摘要： 本文以改性松香（马来松香丙烯酸乙二醇酯）为交联剂，采用表面印迹-悬浮聚合法制备对甲硝唑（MNZ）具有特异选择性的磁性分子印迹聚合物（MMIPs）微粒。首先在以共沉淀法合成的Fe₃O₄钠米粒子（Fe₃O₄ NPs）表面包裹油酸（OA）形成Fe₃O₄@OA NPs；然后，以模板分子甲硝唑、功能单体甲基丙烯酸、交联剂改性松香、Fe₃O₄@OA NPs发生共聚合反应形成MMIPs。通过单因素实验对MMIPs的合成条件进行优化。采用场发射扫描电镜（FESEM）、傅利叶变换红外光谱（FT-IR）、振动样品磁强分析（VSM）、热重分析（TGA）和吸附实验等方法对MMIPs的形态、结构、磁性、热稳定性和分子识别特性等进行表征。结果表明MMIPs的粒径均匀，具有较强热稳定性，快速的磁响应性以及分子识别特异性；在外加磁场作用下，MMIPs可快速将甲硝唑与样品基质分离，大大提高了样品前处理的实验效率。MMIPs作为一种新型固相萃取材料，可以从化妆品样品中选择性分离和富集违规添加的甲硝唑，可应用于化妆品的安全检测。

关键词: 甲硝唑, 磁性分子印迹聚合物, 固相萃取, 改性松香

Abstract: Novel MMIPs were designed and synthesized by surface-suspension polymerization using ethylene glycol maleic rosinate acrylate (EGMRA) as the cross-linking agent in this study. First,oleic acid (OA) was modified onto the surface of Fe₃O₄NPs that were prepared by the co-precipitation. Finally,the MMIP was prepared by suspension polymerization using Fe₃O₄NPs@OA as magnetic core,MNZ as the template molecule,methacrylic acid as the functional monomer,and modified rosin as the cross-linking agent. The optimal synthetic conditions were studied by single factor experiment. The morphology,magnetic,thermal stabilization and adsorption selectivity properties of the obtained MMIPs were characterized by fieldemission scanning electron microscope (SEM),Fourier transform infrared spectrometer (FT-IR),vibrating sample magnetometer (VSM),thermal gravimetric analyzer (TGA) and re-binding experiments. The results indicated that the MMIPs materials had uniformity particle,stronger thermal stabilization,fast magnetism response and high selective adsorption capacity. The absorbed analytes of MMIPs were quickly separated using an external magnetic field which greatly improved sample pre-treatment efficiency. The MMIPs can be used for the separation and enrichment of trace amounts of MNZ in cosmetic samples.

Key words: metronidazole, magnetic molecularly imprinted polymers, solid-phase extraction, modified rosin

中图分类号:

O652.6 TQ314.2

刘敏，吴宗远，李小燕*，王芳，李鹏飞. 以改性松香为交联剂的甲硝唑磁性分子印迹固相萃取材料的制备、表征及分子识别性研究[J]. 天然产物研究与开发, 2016, 28(1): 23-29.

LIU Min,WU Zong-yuan,LI Xiao-yan*,WANG Fang,LI Peng-fei. Synthesis,Characterization and Molecular Recognition Property of Magnetic Molecularly Imprinted Polymers Microspheres with Modified Rosin as Cross-linking agent for Solid Phase Extraction of Metronidazole[J]. NATURAL PRODUCT RESEARCH AND DEVELOPMENT, 2016, 28(1): 23-29.

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以改性松香为交联剂的甲硝唑磁性分子印迹固相萃取材料的制备、表征及分子识别性研究

Synthesis,Characterization and Molecular Recognition Property of Magnetic Molecularly Imprinted Polymers Microspheres with Modified Rosin as Cross-linking agent for Solid Phase Extraction of Metronidazole

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