Abdelshafi Nahla A, Darwish Hany W, Alanazi Ashwag S, Naguib Ibrahim A, Elkhouly Hadeer H, Khodary Nehal S, Mohamed Ekram H
Department of Pharmaceutical Analytical Chemistry, School of Pharmacy, Badr University in Cairo, Badr City, Cairo, 11829, Egypt.
Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, 11451, Riyadh, Saudi Arabia.
BMC Chem. 2024 Mar 6;18(1):48. doi: 10.1186/s13065-024-01146-x.
Pholcodine, an anti-tussive medication widely used as an over-the-counter, OTC drug, has recently faced restrictions in several countries. This paper presents a sensitive electrochemical approach for pholcodine detection. The electrochemical method involved fabricating a graphene nanoplatelets electrode, incorporating polythiophene nanospheres polymer to promote electron transfer and increase the activated surface area. Characterization of the fabricated electrode was performed using transmission electron microscopy, ATR-Fourier-transform infrared spectroscopy, X-ray crystallography, X-ray photoelectron spectroscopy, and electrochemical impedance spectroscopy. The electrochemical behavior of pholcodine with the fabricated electrode was investigated using cyclic voltammetry, chronoamperometry, square wave voltammetry (SWV), and differential pulse voltammetry (DPV). The developed electrode led to a linear response for pholcodine ranging from 10 to 45 mg/L with detection limits of 1.41 and 1.51 mg/mL for SWV and DPV, respectively and quantification limits of 4.27 and 4.57 mg/L for SWV and DPV, respectively. The proposed method has accurately recovered pholcodine in spiked serum samples with a recovery percentage ranging from 1.2 to 2.9%. The optimized method is found to be accurate, precise, and robust by applying validation parameters provided by International Council for Harmonization. Two green metrics were computed to assess the method's greenness, the findings showed that the developed method is environmentally friendly with minimum sample preparation steps.
福尔可定是一种广泛用作非处方药（OTC）的止咳药物，最近在几个国家面临限制。本文提出了一种用于福尔可定检测的灵敏电化学方法。该电化学方法包括制备石墨烯纳米片电极，引入聚噻吩纳米球聚合物以促进电子转移并增加活化表面积。使用透射电子显微镜、衰减全反射傅里叶变换红外光谱、X射线晶体学、X射线光电子能谱和电化学阻抗谱对制备的电极进行表征。使用循环伏安法、计时电流法、方波伏安法（SWV）和差分脉冲伏安法（DPV）研究了福尔可定与制备电极的电化学行为。所开发的电极对福尔可定的线性响应范围为10至45 mg/L，SWV和DPV的检测限分别为1.41和1.51 mg/mL，SWV和DPV的定量限分别为4.27和4.57 mg/L。所提出的方法在加标血清样品中准确回收了福尔可定，回收率在1.2%至2.9%之间。通过应用国际协调理事会提供的验证参数，发现优化后的方法准确、精密且稳健。计算了两个绿色指标以评估该方法的绿色程度，结果表明所开发的方法对环境友好，样品制备步骤最少。
