Lahcen Abdellatif Ait, García-Guzmán Juan José, Palacios-Santander Jose Maria, Cubillana-Aguilera Laura, Amine Aziz
Institute of Research on Electron Microscopy and Materials (IMEYMAT), Department of Analytical Chemistry, Faculty of Sciences, Campus de Excelencia Internacional del Mar (CEIMAR), University of Cadiz, Campus Universitario de Puerto Real, Polígono del Río San Pedro S/N, Puerto Real, Cádiz 11510, Spain; Laboratoire Génie des Procédés & Environnement, Faculté des Sciences et Techniques, Hassan II University of Casablanca, B.P. 146. Mohammedia, Morocco.
Institute of Research on Electron Microscopy and Materials (IMEYMAT), Department of Analytical Chemistry, Faculty of Sciences, Campus de Excelencia Internacional del Mar (CEIMAR), University of Cadiz, Campus Universitario de Puerto Real, Polígono del Río San Pedro S/N, Puerto Real, Cádiz 11510, Spain.
Ultrason Sonochem. 2019 May;53:226-236. doi: 10.1016/j.ultsonch.2019.01.008. Epub 2019 Jan 14.
In this paper, we report for the first time a novel, simple and fast method for the synthesis of magnetic molecularly imprinted polymers (Mag-MIPs) based on high-energy ultrasound probe. Sulfamethoxazole (SMX) was used as template molecule, methacrylic acid as functional monomer, ethylene glycole dimethacrylate as crosslinking agent and magnetic nanoparticles (NPs) as the supporting core. The effects of time (5, 7.5 and 10 min) and the applied amplitude (20, 30, 40, 50 and 60%) using the ultrasound probe for the synthesis of Mag-MIPs were studied and optimized. By applying the proposed synthesis method, the US-magMIPs synthesis time was satisfactorily reduced from several hours to a few minutes (7.5 min) in a simple way. For comparison purposes, the Mag-MIP and the non imprinted polymer (MagNIP) were also synthesized employing an ultrasound bath assisted approach (2 h, 65 °C). Magnetic NPs and US-magMIPs synthesized by both ways were investigated by means of several characterization techniques such as Fourier Transform Infrared (FT-IR) spectroscopy, Scanning/Transmission electron microscopy (SEM and STEM modes), X-Ray Diffraction (XRD), Vibrating Sample Magnetometer (VSM) and Dynamic Light Scattering (DLS). The results obtained confirms clearly the formation of magnetic NPs and their successful decoration by the imprinted polymer in both synthesis ways. The sulfonamide binding efficiency of US-magMIPs synthesized by the ultrasound probe and ultrasound bath were investigated according to the adsorption isotherm. The obtained results showed that the US-magMIP synthesized with the probe has more binding capacity compared to the one synthesized with US bath. The adsorption time was studied and both synthesized US-magMIPs reached the maximum adsorption capacity toward SMX after 1 h and the US-magMIP probe tends to have more easiness to bind SMX in less time. The selectivity studies of the synthesized US-magMIPs based on probe and bath showed a high affinity for SMX compared to its structural analogues such as sulfadiazine, sulfamerazine and sulfacetamide.
在本文中，我们首次报道了一种基于高能超声探头合成磁性分子印迹聚合物（Mag-MIPs）的新颖、简单且快速的方法。以磺胺甲恶唑（SMX）为模板分子，甲基丙烯酸为功能单体，乙二醇二甲基丙烯酸酯为交联剂，磁性纳米粒子（NPs）为支撑核心。研究并优化了使用超声探头合成Mag-MIPs时时间（5、7.5和10分钟）和施加振幅（20、30、40、50和60%）的影响。通过应用所提出的合成方法，以简单的方式将超声Mag-MIPs的合成时间从数小时令人满意地缩短至几分钟（7.5分钟）。为作比较，还采用超声浴辅助方法（2小时，65°C）合成了Mag-MIP和非印迹聚合物（MagNIP）。通过多种表征技术，如傅里叶变换红外（FT-IR）光谱、扫描/透射电子显微镜（SEM和STEM模式）、X射线衍射（XRD）、振动样品磁强计（VSM）和动态光散射（DLS），对两种方法合成的磁性纳米粒子和超声Mag-MIPs进行了研究。所得结果清楚地证实了在两种合成方式中均形成了磁性纳米粒子及其被印迹聚合物成功修饰。根据吸附等温线研究了超声探头和超声浴合成的超声Mag-MIPs对磺胺类药物的结合效率。所得结果表明，与超声浴合成的超声Mag-MIP相比，探头合成的超声Mag-MIP具有更高的结合能力。研究了吸附时间，两种合成的超声Mag-MIPs在1小时后对SMX均达到最大吸附容量，且超声Mag-MIP探头在更短时间内更易于结合SMX。基于探头和浴合成的超声Mag-MIPs的选择性研究表明，与磺胺嘧啶、磺胺甲嘧啶和磺胺醋酰等结构类似物相比，其对SMX具有高亲和力。
