Department of Chemistry, Faculty of Science, Yazd University, 89195-741, Yazd, Iran.
Renewable Energies Research Laboratory, Department of Chemistry, Faculty of Science, University of Sistan and Baluchestan, P.O. Box 98135 674, Zahedan, Iran.
Mikrochim Acta. 2023 Mar 29;190(4):164. doi: 10.1007/s00604-023-05746-7.
A magnetic molecularly imprinted polymer (MMIP) was fabricated for captopril by surface polymerization of FeO@SiO nanoparticles using a new functional monomer of N-(allylcarbamothioyl)-2-chlorobenzamide. It was then employed as a selective nanosorbent for dispersive magnetic micro solid phase extraction (DM-μ-SPE) of captopril from biological and wastewater samples. To characterize the physicochemical properties of the MMIP, different analytical methods such as the vibrating sample magnetometer, field emission scanning electron microscopy, Brunauer-Emmett-Teller, and Fourier transform infrared spectroscopy were utilized. To gain the maximum extraction recovery of captopril, the influence of various operating conditions was investigated and experimental settings optimized. After the extraction step, the concentration of captopril was measured by UV-Vis spectrophotometer at 245 nm. The assessments demonstrated that the MMIP provides higher extraction efficiency in comparison to magnetic non-imprinted polymer, suggesting the establishment of selective recognition binding sites at the MMIP surface. The method depicted desirable figures of merit of a low detection limit of 0.16 μg L, a limit of quantification of 0.50 μg L, a linear dynamic range of 0.50-22.0 μg L, and an acceptable preconcentration factor of 333. The magnetic MIP was successfully employed for preconcentration and extraction of trace amounts of captopril in real samples, such as human blood serum, urine, and wastewater samples, with recoveries in the range 95.7 to 102.6% and relative standard deviations < 5%.
采用 FeO@SiO 纳米粒子表面聚合，以 N-(丙烯酰基氨硫酰基)-2-氯苯甲酰胺为功能单体，制备了卡托普利磁性分子印迹聚合物（MMIP）。然后，它被用作从生物和废水样品中选择性分散磁性微固相萃取（DM-μ-SPE）卡托普利的纳米吸附剂。为了表征 MMIP 的物理化学性质，使用了振动样品磁强计、场发射扫描电子显微镜、Brunauer-Emmett-Teller 和傅里叶变换红外光谱等不同的分析方法。为了获得卡托普利的最大萃取回收率，研究了各种操作条件的影响，并对实验条件进行了优化。萃取步骤后，在 245nm 处用紫外-可见分光光度计测量卡托普利的浓度。评估表明，与磁性非印迹聚合物相比，MMIP 提供了更高的萃取效率，表明在 MMIP 表面建立了选择性识别结合位点。该方法表现出理想的评价指标，检出限低至 0.16μg/L，定量限低至 0.50μg/L，线性动态范围为 0.50-22.0μg/L，可接受的预浓缩因子为 333。该磁性 MIP 成功用于实际样品中痕量卡托普利的预浓缩和萃取，如人血清、尿液和废水样品，回收率在 95.7%至 102.6%之间，相对标准偏差 <5%。
