核-壳型没食子蓝磁性分子印迹固相萃取材料的合成、表征及应用研究  

Preparation and absorption performance of core-shell magnetic molecularly imprinted polymer microspheres for solid phase extraction and detection of Gallocyanine in foods

作　　者：苏晓濛[1] 李小燕[1] 刘敏[1] 吴宗远[1] 

机构地区：[1]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,南宁530008

出　　处：《食品科技》2014年第12期332-339,共8页Food Science and Technology

基　　金：国家自然科学基金项目(21165003)

摘　　要：采用化学共沉淀法制备Fe3O4磁性纳米粒子,以3-氨丙基三乙氧基硅烷（APTES）对其表面进行氨基硅烷化改性,形成Fe3O4@SiO2-NH2纳米粒子。以其作为磁性核,采用表面印迹技术,以没食子蓝为模板,丙烯酰胺（AM）为功能单体,乙二醇二甲基丙烯酸酯（EGDMA）为交联剂,在Fe3O4@SiO2-NH2表面形成没食子蓝分子印迹聚合膜,制备了核-壳型没食子蓝磁性分子印迹聚合物（Fe3O4@MIPs）。分别采用红外光谱（FT-IR）、场发射扫描电镜（FESEM）、振动样品磁强分析（VSM）和热重分析（TGA）等仪器分析手段,对Fe3O4@MIPs的结构进行表征。研究了它对没食子蓝的吸附性能,探讨了吸附动力学、吸附等温线及分子识别性。并将其应用于食品中分离富集没食子蓝。结果表明,所制备的核-壳型磁性分子印迹聚合物具有高吸附容量（表观最大吸附量达149.32 mg/g）,快速的结合动力学（60 min达吸附平衡）及显著的吸附选择性（印迹因子达9.10）。以其作为新型固相萃取材料,结合高效液相色谱（HPLC）检测,对加标食品样品中的没食子蓝进行分离、纯化、检测,加标回收率在97.69%-104.4%之间,RSD在0.85%-1.2%之间,检测限为0.0051μg/m L。在外加磁场作用下Fe3O4@MIPs可快速与样品基质分离,大大提高了实验效率。该方法简单快速,可应用于食品中非法添加的没食子蓝的分离检测。Fe3O4 magnetic nanoparticles were synthesized by the chemical co-precipitation method. With（3-aminopropyl） triethoxysilane（APTES） on the surface modification, Fe3O4@SiO2-NH2 nanoparticles were formed. Core-shell magnetic molecularly imprinted polymers（Fe3O4@MIPs） were prepared by using Gallocyanine as template molecule, acrylamide（AM） as functional monomer, ethyleneglycol dimethacrylate（EGDMA） as cross-linking agent, and amino-modified Fe3O4 magnetic nanoparticles as the magnetic core. The Fe3O4@MIPs were characterized using a Fourier transform infrared spectrometer（FTIR）, field emission scanning electron microscope（FESEM）, vibrating sample magnetometer（VSM）, and thermogravimetric analysis（TGA）. The Fe3O4@MIPs were studied by the re-binding experiments, such as adsorption kinetics, adsorption isotherm, molecular identifi cation, and applied to the separation and enrichment of Gallocyanine in food. The results showed that the core-shell Fe3O4@MIPs has a fast adsorption equilibrium, highly improved imprinting capacity and significant selectivity; the recoveries were in the range of 97.69%-104.4%, the relative standard deviation was 0.85%-1.2%, and the detection limit was 0.0051 μg/m L（S/N=3）. Under the action of additional magnetic field, the polymers can be quickly separated from the sample matrix, greatly improve the efficiency of experiments. So the coreshell Fe3O4@MIPs could be used as a solid-phase extraction material and detect the illegal addition of Gallocyanine in food conveniently.

关 键 词：核-壳型 磁性分子印迹聚合物 固相萃取 没食子蓝 

分 类 号：O658.2[理学—分析化学]