Turbale Mahilet, Moges Amsalu, Dawit Mulugeta, Amare Meareg
Samara University, Ethiopia.
Debre Markos University, Ethiopia.
Heliyon. 2020 Dec 23;6(12):e05782. doi: 10.1016/j.heliyon.2020.e05782. eCollection 2020 Dec.
A selective and sensitive electrochemical method based on glassy carbon electrode modified with poly(malachite green) was developed for determination of tetracycline in pharmaceutical capsule formulation. Cyclic voltammetry and electrochemical impedance spectroscopy using [Fe(CN)] as a probe were used to characterize the potentiodynamiclly deposited poly(malachite green) on the surface of glassy carbon electrode. In contrast to the unmodified glassy carbon electrode, the fabricated poly(malachite green) modified glassy carbon electrode showed catalytic property towards two steps irreversible oxidation of tetracycline. Better correlation of the oxidative peak current with the scan rate than with the square root of scan rate supported by slope of 0.60 for log(current) versus log(scan rate) indicated that the oxidation reaction of tetracycline at the modified electrode was predominantly controlled by electron exchange step at the solution polymer interface. Under optimized solution pH, and accumulation parameters, the square wave adsorptive anodic striping peak current response of the modified electrode showed linear dependence on concentration of tetracycline in the range 5-100 μM with determination coefficient, method detection limit, and quantification limit of 0.99588, 1.6 μM, and 5.3 μM, respectively. The tetracycline content of a capsule sample claimed to have 250 mg/capsule was found to be 250.53 mg/capsule with 0.21% deviation. Excellent spike recovery result of 99.80%, and 98.49-99.78% recovery of tetracycline in capsule sample in the presence of 50-200% of UA, AA, and ampicillin validated the applicability of the method for determination of tetracycline in real samples with complex matrix like capsule formulations.
开发了一种基于聚(孔雀石绿)修饰玻碳电极的选择性和灵敏的电化学方法,用于测定药物胶囊制剂中的四环素。使用[Fe(CN)]作为探针的循环伏安法和电化学阻抗谱用于表征在玻碳电极表面电位动力学沉积的聚(孔雀石绿)。与未修饰的玻碳电极相比,制备的聚(孔雀石绿)修饰玻碳电极对四环素的两步不可逆氧化表现出催化性能。氧化峰电流与扫描速率的相关性优于与扫描速率平方根的相关性,log(电流)对log(扫描速率)的斜率为0.60,这表明四环素在修饰电极上的氧化反应主要受溶液-聚合物界面电子交换步骤的控制。在优化的溶液pH值和富集参数下,修饰电极的方波吸附阳极溶出伏安峰电流响应与四环素浓度在5-100μM范围内呈线性关系,测定系数、方法检出限和定量限分别为0.99588、1.6μM和5.3μM。一个声称每粒含250mg的胶囊样品中四环素含量为250.53mg/胶囊,偏差为0.21%。在存在50-200%的尿酸、抗坏血酸和氨苄青霉素的情况下,胶囊样品中四环素的加标回收率极佳,为99.80%,回收率为98.49-99.78%,验证了该方法在测定胶囊制剂等复杂基质实际样品中四环素的适用性。