Noureldin Hind A M, Abdel-Aziz Ali M, Mabrouk Mokhtar M, Saad Amira H K, Badr Ibrahim H A
Department of Analytical Chemistry, Faculty of Pharmacy, Badr University in Cairo Cairo Egypt.
Department of Chemistry, Faculty of Science, Ain Shams University Cairo Egypt
RSC Adv. 2023 Jan 3;13(2):844-852. doi: 10.1039/d2ra06768d.
A simple, cost-effective, and efficient differential pulse voltammetric (DPV) assay for monitoring spiramycin adipate (SPA) in its dosage forms, urine, and milk samples at an activated glassy carbon electrode (GCE) was developed. GCE was electrochemically activated by anodization at a high positive voltage (2.5 V). The activated glassy carbon electrode (AGCE) was surface characterized, optimized, and utilized for the electrochemical assay of SPA. The electrochemical behavior of the AGCEs was investigated using cyclic voltammetry (CV) which shows a remarkable increase in the anodic peak of SPA in comparison with GCE. This behavior reflects a remarkable increase in the electrocatalytic oxidation of SPA at AGCE. The impacts of various parameters such as scan rate, accumulation time, and pH were investigated. The analytical performance of the activated glassy carbon electrodes was studied utilizing DPV. Under optimum conditions, the oxidation peak current exhibited two linear ranges of 80 nm to 0.8 μM and 0.85-300 μM with a lower limit of detection (LOD) of 20 nM. The developed assay exhibited high sensitivity, excellent repeatability, and good selectivity. Additionally, the developed SPA-sensitive modified GCE was successfully applied for SPA assay in its pharmaceutical dosage form and diluted biological fluids as well, with satisfactory recovery results which correlated well with the results obtained using spectrophotometry.
开发了一种简单、经济高效的差分脉冲伏安法(DPV),用于在活化玻碳电极(GCE)上监测己二酸螺旋霉素(SPA)在其剂型、尿液和牛奶样品中的含量。通过在高正电压(2.5 V)下进行阳极氧化对GCE进行电化学活化。对活化玻碳电极(AGCE)进行表面表征、优化,并将其用于SPA的电化学检测。使用循环伏安法(CV)研究了AGCE的电化学行为,结果表明与GCE相比,SPA的阳极峰有显著增加。这种行为反映了AGCE上SPA的电催化氧化有显著增加。研究了扫描速率、富集时间和pH等各种参数的影响。利用DPV研究了活化玻碳电极的分析性能。在最佳条件下,氧化峰电流呈现出80 nM至0.8 μM和0.85 - 300 μM两个线性范围,检测下限(LOD)为20 nM。所开发的检测方法具有高灵敏度、出色的重复性和良好的选择性。此外,所开发的对SPA敏感的修饰GCE也成功应用于其药物剂型和稀释生物流体中SPA的检测,回收率结果令人满意,与分光光度法获得的结果相关性良好。