Department of Chemistry, Faculty of Science, Damietta University, New Damietta 34517, Egypt.
Comb Chem High Throughput Screen. 2020;23(10):1002-1009. doi: 10.2174/1386207323666200422083339.
The development of easy, accurate, reliable technique which is characterized by low cost, minimal sample pre-treatment, and short analysis time to monitor RFX residues in milk samples before distribution to consumers.
Literature survey reveals several analytical methods, including high-performance liquid chromatography (HPLC), ultra-performance liquid chromatography (UPLC) and thin-layer chromatography (TLC)-densitometry. These methods are time consuming, require additional steps like preconcentration or multisolvent extraction, trained technicians, and expensive instruments.
The electrochemical analysis of RFX was effectively established by the adsorptive stripping method on GCE due to the effective interfacial accumulation of RFX on the electrode surface. The RFX adsorptive accumulation is followed by electrochemical measurement of the accumulated analyte.
The electrochemical oxidation of RFX was studied at glassy carbon electrodes (GCE) in Britton-Robinson buffer (BR) solutions over the pH range from 2.0-12.0 using cyclic and differential pulse voltammetry (DPV). The oxidation of the drug was accomplished in a single irreversible, adsorption-controlled step within the pH range 4.0-9.0. Therefore, the application of GCE for a sensitive and selective quantification of RFX by adsorptive stripping voltammetry was reported. This format was satisfactorily applied for the determination of RFX in bovine milk. Limit of detection (LOD) of 1.25 μg kg-1 of milk and mean recoveries of 97.8 to 107.5% were achieved.
The proposed method might be competitive with the HPLC techniques. The detection limit found for RFX on GCE for milk samples, after medium exchange, was well below the MRLs, the maximum concentration of a veterinary drug residue legally permissible in food, are proposed by the European Medicines Agency.
开发一种简单、准确、可靠的技术,该技术具有成本低、样品预处理简单、分析时间短的特点,可用于监测在分发给消费者之前牛奶样品中的 RFX 残留。
文献调查显示,有几种分析方法,包括高效液相色谱法(HPLC)、超高效液相色谱法(UPLC)和薄层色谱法(TLC)-密度法。这些方法耗时,需要额外的步骤,如预浓缩或多溶剂提取、培训技术人员和昂贵的仪器。
由于 RFX 在电极表面的有效界面积累,通过吸附剥离法在 GCE 上有效地建立了 RFX 的电化学分析。在电极表面上吸附积累 RFX 后,对积累的分析物进行电化学测量。
在 Britton-Robinson 缓冲液(BR)溶液中,在玻璃碳电极(GCE)上研究了 RFX 的电化学氧化,使用循环伏安法和差分脉冲伏安法(DPV)在 pH 值 2.0-12.0 范围内进行测量。在 pH 值 4.0-9.0 范围内,药物的氧化是在单个不可逆、吸附控制步骤内完成的。因此,报道了 GCE 用于通过吸附剥离伏安法对 RFX 进行灵敏和选择性定量的应用。这种格式被满意地应用于牛奶中 RFX 的测定。在牛奶中检测到的 RFX 的检出限(LOD)为 1.25μg kg-1,平均回收率为 97.8%至 107.5%。
所提出的方法可能与 HPLC 技术具有竞争力。在进行介质交换后,GCE 对牛奶样品中的 RFX 的检测限远低于欧洲药品管理局提出的最大残留限量(MRL),即食品中允许的兽用药物残留的最大浓度。