摘要
制备了一种新型核-壳型的磁性固相萃取材料MGTPⅠ(内核为Fe3O4@GO@Si O2(MGT)纳米粒子,丙烯酸-乙二醇二甲基丙烯酸酯共聚物(AA-EGDMA)为壳)。分别采用扫描电镜(SEM),红外分析(FT-IR),振动样品磁强分析(VSM),热重分析(TGA)对MGTPⅠ的形貌,结构,磁化性能,热稳定性等进行表征。用静态吸附实验对MGTPⅠ进行了吸附热动力学研究,并进行吸附模型的判断。结果表明,所制备的核-壳型磁性聚合物具有较快的结合动力学(60 min可达吸附平衡),较高的吸附性能(最大表观吸附量达89.53 mg/g)。将其应用于降糖保健品中(降糖颗粒、降糖片、降糖茶)甲苯磺丁脲的检测,回收率分别为88.91%~95.20%,81.63%~107.49%,92.10%~102.99%,RSD≤2.53%,检测限为0.15μg/m L,展现了良好的精密度和准确性。且MGTPⅠ可以至少重复使用四次,具有良好的耐用性。在外加磁场作用下可快速的对目标物进行分离、富集,有望应用于降糖保健品中甲苯磺丁脲的安全检测。
Core-shell magnetic polymers (MGTP I )were prepared by using acrylic acid (AA)as functional monomer, ethyleneglycol dimethacrylate (EGDMA) as cross - linking agent, and hydroxy - modified MGT nanoparticles as the magnetic core.Morphology, structure, magnetic properties,thermal stability of MGTP I were characterized by scanning electron microscopy ( SEM ), fourier transform infrared spectroscopy ( FTIR), vibrating sample strong magnetic analysis ( VSM ), thermogravimetric analysis (TGA) . Re - binding experiments were undertaken for the study of the adsorption thermodynamic and kinetic,which could make sure adsorption model of the materials.The results showed that the MGTP I had a fast adsorption equilibrium ( adsorption equilibrium time was just 60 min)and nice adsorption capacity (the max adsorption was 89.53 mg/g).The MGTP I could be applied to the enrichment and determination of tolbutamide in hypoglycemic health products with the recoveries of spiked hypoglycemic granule, hypoglycemic tablets, and hypoglycemic tea ranging from 88.91% to 95.20%, 81.63% to 107.49% ,and 92.10% to 102.99% ,respectively,and the RSD was ≤2.53% ,the limit of detection( LOD)was 0.15 μg/mL. The durability test showed that the MGTP I could be reused more than 4 times by re-binding experiments.By using an external magnetic field, the absorbed analytes were efficiently separated, so it was a promising method to conveniently detect the illegal addition of tolbutamide in hypoglycemic health products.
出处
《食品工业科技》
CAS
CSCD
北大核心
2016年第18期49-54,59,共7页
Science and Technology of Food Industry
基金
国家自然科学基金项目(21165003
21545011)
关键词
核-壳型磁性聚合物
固相萃取
甲苯磺丁脲
保健品
core-shell magnetic polymer
solid phase extraction
tolbutamide
hypoglycemic health products