核-壳型磁性固相萃取材料对降糖保健品中甲苯磺丁脲吸附性能的研究

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。 

Synthesis and absorption performance of core- shell magnetic polymer materials for solid phase extraction and detection of Tolbutamide in hypoglycemic health products

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 MGTPⅠ 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 MGTPⅠ 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) was0.15 μg / m L. 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.