Polymers and Pigments Department, National Research Centre, Dokki, P.O. Box 12622, Giza, Egypt.
Applied Organic Chemistry Department, National Research Centre, Dokki, P.O. Box 12622, Giza, Egypt.
Int J Biol Macromol. 2024 Nov;280(Pt 4):136022. doi: 10.1016/j.ijbiomac.2024.136022. Epub 2024 Sep 25.
In current research, an innovative pectic acid was grafted with poly (acrylamide-co-acrylic acid) [PA-g-poly (AAm-co-AA)] nanoporous membrane using a free radical-mediated grafting copolymerization process. The optimized parameters for the grafting copolymerization reaction such as initiator concentration, monomer concentrations, polymerization reaction time, and temperature were studied. Additionally, the solid content, graft percentage, and conversion were calculated. The unique polymeric membrane was characterized using Fourier-transform infrared spectroscopy (FT-IR), thermal gravimetry (TG), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) supported by energy dispersive X-ray spectroscopy (EDX). The formulated novel PA-g-poly (AAm-co-AA) had a nanoporous structure with a diameter of 113 nm. pH-dependent swelling and biodegradation measurements were also studied. The electrochemical characterizations of PA-g-poly (AAm-co-AA) were conducted through cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Furthermore, the screen-printed electrode (SPE) was modified with pure PA and the new generation of its grafted polymeric nanoparticles to detect and quantify the concentration of riboflavin (RF) in real samples using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques. The modified electrode showed two linear concentration ranges from 0.01 - 2 nM and 2 - 90 nM with low detection limits (LODs) of 0.004 and 0.97 nM, respectively, demonstrating high sensitivity. Besides, the fabricated sensor exhibited more selectivity, simplicity, great reproducibility, repeatability, and good stability. Finally, the PA-g-poly (AAm-co-AA)-modified SPE based sensor was effectively used in real sample analysis of egg yolk, milk, and vitamin B2 drugs with good recovery rates.
在当前的研究中,采用自由基介导的接枝共聚反应,将一种创新的果胶接枝到聚(丙烯酰胺-共-丙烯酸)[PA-g-poly(AAm-co-AA)]纳米多孔膜上。研究了接枝共聚反应的优化参数,如引发剂浓度、单体浓度、聚合反应时间和温度。此外,还计算了固含量、接枝率和转化率。利用傅里叶变换红外光谱(FT-IR)、热重分析(TG)、透射电子显微镜(TEM)和扫描电子显微镜(SEM)结合能谱(EDX)对独特的聚合物膜进行了表征。所制备的新型 PA-g-poly(AAm-co-AA)具有纳米多孔结构,直径为 113nm。还研究了 pH 值依赖性溶胀和生物降解。通过循环伏安法(CV)和电化学阻抗谱(EIS)对 PA-g-poly(AAm-co-AA)进行了电化学表征。此外,通过循环伏安法(CV)和差分脉冲伏安法(DPV)技术,将纯 PA 和新一代接枝聚合物纳米颗粒修饰在丝网印刷电极(SPE)上,用于检测和定量实际样品中核黄素(RF)的浓度。修饰后的电极显示出两个线性浓度范围,分别为 0.01-2 nM 和 2-90 nM,检测限(LOD)分别为 0.004 和 0.97 nM,表现出高灵敏度。此外,所制备的传感器表现出更高的选择性、简单性、良好的重现性、重复性和稳定性。最后,基于 PA-g-poly(AAm-co-AA)的修饰的 SPE 传感器有效地用于蛋黄、牛奶和维生素 B2 药物的实际样品分析,回收率良好。