University of Zagreb, Faculty of Pharmacy and Biochemistry, A. Kovacica 1, 10000 Zagreb, Croatia.
University of Zagreb, Faculty of Pharmacy and Biochemistry, A. Kovacica 1, 10000 Zagreb, Croatia.
Talanta. 2016 Jan 15;147:50-8. doi: 10.1016/j.talanta.2015.09.036. Epub 2015 Sep 16.
A rapid analytical method without the time-consuming separation step was developed to simultaneously determine mesalazine and its N-acetylated metabolite. A simply designed electrochemical sensor with functionalized carbon nanotubes in a Nafion matrix was constructed for this purpose. The presence of the nanocomposite modifier on the electrode surface significantly affects the voltammetric response of target analytes. The morphology of the modified surface was investigated by scanning electron microscopy. The effect of modifier amount on the sensor performance was investigated in order to obtain the most favorable response of mesalazine since it was found in lower concentration limits in real samples then its metabolite due to the rapid drug elimination and the slightly slower renal metabolite excretion. Under optimal conditions, the anodic peak currents measured by square-wave voltammetry increased linearly after short accumulation of 30s in the range of 5.0×10(-8)-2.5×10(-6)M and 1.0×10(-7)-5.0×10(-6)M for drug and metabolite, respectively. In addition to stable response, the sensor has excellent performance associated with high sensitivity (2.33×10(7) and 8.37×10(6)µAM(-1) for drug and metabolite, respectively). The synergistic effect of the carbon nanotubes and Nafion polymer film yielded detection limit of 1.2×10(-8)M for mesalazine and 2.6×10(-8)M for its metabolite that is comparable to known chromatographic methods. Due to the easy preparation and regeneration, the proposed sensor opens new opportunity for fast, simple and sensitive analysis of drug and its metabolite in human serum samples as well as direct quantification of mesalazine in delayed-release formulations.
开发了一种无需耗时分离步骤的快速分析方法,以同时测定美沙拉嗪及其 N-乙酰化代谢物。为此,构建了一个简单设计的电化学传感器,其在 Nafion 基质中具有功能化的碳纳米管。纳米复合材料修饰剂在电极表面的存在显着影响目标分析物的伏安响应。通过扫描电子显微镜研究了修饰表面的形态。为了获得美沙拉嗪的最佳响应,研究了修饰剂用量对传感器性能的影响,因为与代谢物相比,它在真实样品中的浓度限制较低,因为药物消除迅速,而肾脏代谢物排泄稍慢。在最佳条件下,在 5.0×10(-8)-2.5×10(-6)M 和 1.0×10(-7)-5.0×10(-6)M 范围内,通过方波伏安法测量的阳极峰电流在 30s 的短时间积累后呈线性增加,分别为药物和代谢物。除了稳定的响应外,传感器还具有与高灵敏度相关的出色性能(药物和代谢物分别为 2.33×10(7)和 8.37×10(6)µAM(-1))。碳纳米管和 Nafion 聚合物膜的协同作用使美沙拉嗪的检测限达到 1.2×10(-8)M,其代谢物的检测限达到 2.6×10(-8)M,与已知的色谱方法相当。由于制备和再生简单,因此该传感器为在人血清样品中快速、简单和灵敏地分析药物及其代谢物以及直接定量延迟释放制剂中的美沙拉嗪提供了新的机会。