College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, PR China; Key Laboratory of Hunan Province for Water Environment and Agriculture Product Safety, Central South University, Changsha 410083, PR China.
College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, PR China; Hunan Provincial Key Laboratory of Efficient and Clean Utilization of Manganese Resources, Central South University, Changsha 410083, Hunan, China.
Talanta. 2019 Mar 1;194:969-976. doi: 10.1016/j.talanta.2018.10.099. Epub 2018 Oct 30.
Hydrophilic magnetic molecular imprinted resins (MMIRs) were firstly fabricated by one-pot copolycondensation of resorcinol, melamine, and formaldehyde in the pores of FeO @mSiO. The porous structure of mSiO limited copolycondensation. After the removal of mSiO, controllable imprinting shell thickness (about 5 nm) was formed, reducing the probability of embedded sites, favoring the efficient adsorption. Moreover, the reaction time (3 h) was just 1/5-1/8 of those synthesized by conventional heating method. The transmission electron microscopy (TEM), Fourier transform infrared (FT-IR), vibrating sample magnetometer (VSM), thermo-gravimetric analysis (TGA), water contact angle analysis, and Brunauer‒Emmett‒Teller (BET) analysis indicated the successful preparation of MMIRs with excellent hydrophilic property, and magnetic separation characteristics. Steady-state adsorption studies showed that the resultant MMIRs had specific recognition for benzoic acids, GA, protocatechuic acid (PCA), vanillic acid (VA), 4-hydroxybenzoic acid (4-HBA), salicylic acid (SA), and benzoic acid (BA). MMIRs combination with high-performance liquid chromatography-ultraviolet (HPLC-UV) were then directly used for selective extraction and determination of benzoic acids in river water, fruit juices, and human serum. Obtained limits of detection (LOD) and recoveries were in the range of 0.02-1.0 μg/mL, and 81.8-108.7%, respectively, and the batch-to-batch relative standard deviation (RSD) was 5.9%. The proposed strategy showed excellent hydrophilicity and specificity, which was promising for detection of benzoic acids in real aqueous samples.
亲水磁性分子印迹树脂(MMIRs)首次通过在 FeO@mSiO 孔中进行间苯二酚、三聚氰胺和甲醛的一锅共聚缩合合成。mSiO 的多孔结构限制了共聚缩合。mSiO 去除后,形成了可控的印迹壳厚度(约 5nm),降低了嵌入位的概率,有利于高效吸附。此外,反应时间(3h)仅为传统加热法的 1/5-1/8。透射电子显微镜(TEM)、傅里叶变换红外(FT-IR)、振动样品磁强计(VSM)、热重分析(TGA)、水接触角分析和 Brunauer-Emmett-Teller(BET)分析表明,成功制备了具有优异亲水性能和磁分离特性的 MMIRs。稳态吸附研究表明,所得 MMIRs 对苯甲酸、GA、原儿茶酸(PCA)、香草酸(VA)、4-羟基苯甲酸(4-HBA)、水杨酸(SA)和苯甲酸(BA)具有特异性识别。然后,将 MMIRs 与高效液相色谱-紫外(HPLC-UV)结合,直接用于河水、果汁和人血清中苯甲酸的选择性提取和测定。获得的检测限(LOD)和回收率分别在 0.02-1.0μg/mL 和 81.8-108.7%范围内,批间相对标准偏差(RSD)为 5.9%。该策略表现出优异的亲水性和特异性,有望用于实际水样中苯甲酸的检测。