Magar Hend S, Fahim Asmaa M, Hashem M S
Applied Organic Chemistry Department, National Research Centre Dokki, P. O. Box. 12622 Giza Egypt
Department of Green Chemistry, National Research Centre Dokki, P. O. Box. 12622 Giza Egypt.
RSC Adv. 2024 Dec 17;14(54):39820-39832. doi: 10.1039/d4ra06271j.
In this study, we demonstrated how to design and construct a highly specific and sensitive sensor capable of rapidly and accurately detecting ascorbic acid (AA). A sulfonamide derivative (S) acting as a novel monomer was synthesized through an aldol condensation reaction. Subsequently, a free radical-mediated grafting polymerization approach was used to create a new generation of gelatin (Gel) grafted with poly sulfonamide derivative (Gel-g-PS). The graft percentage (GP%) was 60 ± 0.5% with a conversion rate of 98.3%. Fourier-transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM) were utilized to confirm the formation of Gel-g-PS. The developed gelatin sulfonamide modified screen printed electrode (Gel-g-PS/SPE) was employed for the determination of ascorbic acid (AA) in fruit juices and pharmaceutical samples. Gel-g-PS/SPE showed excellent electrochemical catalytic activities toward AA oxidation compared to bare (unmodified) SPE. Ascorbic acid displayed a sensitive oxidation peak at 0.35 V using the differential pulse voltammetry technique. Under optimized experimental conditions, the two linear ranges for AA detection were obtained to be from 0.2-5 ppb and 20-600 ppb, with a limit of detection (LoD) of 0.03 ppb and a limit of quantification (LoQ) of 0.11 ppb. The proposed Gel-g-PS modified SPE surface demonstrated good selectivity, stability, reproducibility, and repeatability as well as a good recovery rate in fresh fruit juices and pharmaceutical samples.
在本研究中,我们展示了如何设计和构建一种能够快速、准确检测抗坏血酸(AA)的高特异性和高灵敏度传感器。通过羟醛缩合反应合成了一种作为新型单体的磺酰胺衍生物(S)。随后,采用自由基介导的接枝聚合方法制备了新一代接枝有聚磺酰胺衍生物的明胶(Gel-g-PS)。接枝率(GP%)为60±0.5%,转化率为98.3%。利用傅里叶变换红外光谱(FT-IR)和扫描电子显微镜(SEM)来确认Gel-g-PS的形成。所开发的明胶磺酰胺修饰丝网印刷电极(Gel-g-PS/SPE)用于测定果汁和药物样品中的抗坏血酸(AA)。与裸(未修饰)SPE相比,Gel-g-PS/SPE对AA氧化表现出优异的电化学催化活性。使用差分脉冲伏安法技术,抗坏血酸在0.35 V处显示出一个灵敏的氧化峰。在优化的实验条件下,获得了AA检测的两个线性范围为0.2 - 5 ppb和20 - 600 ppb,检测限(LoD)为0.03 ppb,定量限(LoQ)为0.11 ppb。所提出的Gel-g-PS修饰SPE表面在新鲜果汁和药物样品中表现出良好的选择性、稳定性、重现性和重复性以及良好的回收率。