Brycht Mariola, Nosal-Wiercińska Agnieszka, Sipa Karolina, Rudnicki Konrad, Skrzypek Sławomira
Department of Inorganic and Analytical Chemistry Faculty of Chemistry, University of Lodz, Tamka 12, 91-403 Lodz, Poland.
Department of Analytical Chemistry and Instrumental Analysis Faculty of Chemistry, Maria Skłodowska-Curie University, M. Skłodowska-Curie sq. 3, 20-031 Lublin, Poland.
Monatsh Chem. 2017;148(3):463-472. doi: 10.1007/s00706-016-1862-z. Epub 2016 Oct 28.
In this paper, the square-wave adsorptive stripping voltammetric (SWAdSV) determination of the veterinary drug closantel using a renewable silver amalgam film electrode (Hg(Ag)FE) is presented. As observed in SWAdSV, closantel provided one well-shaped reduction peak suitable for analytical purposes at potential ca. -1.4 V in the Britton-Robinson (B-R) buffer at pH 7.0. At optimal conditions, the SWAdSV response of Hg(Ag)FE for determining closantel was linear over two concentration ranges of 5.0 × 10 to 2.0 × 10 mol dm and 2.0 × 10 to 1.2 × 10 mol dm with a detection limit of 1.1 × 10 mol dm. In addition, a relevance of the developed SWAdSV method was successfully verified by the quantitative analysis of closantel in the commercial formulation Closamectin Pour-On with satisfactory results (RSD = 5.8%, recovery = 101.8%). The results showed that the developed procedure can be adequate for screening purposes. Also, the electrochemical behavior of closantel was characterized by cyclic voltammetry, and it was found that closantel exhibited a quasi-reversible behavior with cathodic peak on the forward scan at ca. -1.4 V and anodic peak on the reverse scan at ca. -1.35 V vs. Ag/AgCl in B-R buffer, pH 7.0. As the obtained results showed that the electrode mechanism of closantel is controlled by the adsorption, the effect of adsorption was studied using the electrochemical impedance spectroscopy technique.
本文介绍了使用可再生银汞膜电极(Hg(Ag)FE)通过方波吸附溶出伏安法(SWAdSV)测定兽药氯氰碘柳胺。如在SWAdSV中观察到的,在pH 7.0的 Britton-Robinson(B-R)缓冲液中,氯氰碘柳胺在约-1.4 V的电位下提供了一个适合分析目的的形状良好的还原峰。在最佳条件下,Hg(Ag)FE用于测定氯氰碘柳胺的SWAdSV响应在5.0×10至2.0×10 mol dm和2.0×10至1.2×10 mol dm的两个浓度范围内呈线性,检测限为1.1×10 mol dm。此外,通过对商业制剂氯氰碘柳胺浇泼剂中氯氰碘柳胺的定量分析成功验证了所开发的SWAdSV方法的相关性,结果令人满意(相对标准偏差=5.8%,回收率=101.8%)。结果表明,所开发的方法可适用于筛选目的。此外,通过循环伏安法对氯氰碘柳胺的电化学行为进行了表征,发现在pH 7.0的B-R缓冲液中,相对于Ag/AgCl,氯氰碘柳胺表现出准可逆行为,正向扫描时在约-1.4 V处有阴极峰,反向扫描时在约-1.35 V处有阳极峰。由于所得结果表明氯氰碘柳胺的电极机理受吸附控制,因此使用电化学阻抗谱技术研究了吸附的影响。