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

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

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.