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Poly(bis(2,2′-bipyridine) hydroxy Copper(II) iodide modified glassy carbon electrode for electrochemical determination of chloroquine in pharmaceuticals and biological samples
Sensing and Bio-Sensing Research Pub Date : 2023-10-18 , DOI: 10.1016/j.sbsr.2023.100598
Mulu Gashu , Belete Asefa Aragaw , Molla Tefera , Atakilt Abebe

A new electrochemical sensor, poly(bis(2,2′-bipyridine)hydroxycopper(II) iodide modified glassy carbon electrode (poly([Cu(Bip)2OH]I)/GCE), was prepared by electropolymerization of bis(2,2′-bipyridine)chlorocopper(II) iodide ([Cu(Bip)2Cl]I) on glassy carbon electrode (GCE) for voltammetric determination of chloroquine (CQ). The synthesized complex (bis(2,2′-bipyridine)chlorocopper(II) iodide) was characterized using UV–Vis, CHN elemental analysis, atomic absorption spectroscopy (AAS), electrolytic conductivity, melting point and Fourier transform infrared spectroscopy (FT-IR) were used to characterize and confirm the synthesis of the desired complex (bis(2,2′-bipyridine)chlorocopper(II) iodide). The Uv-Vis, FTIR and electrochemical data of the synthesized polymer supports the replacement of chloro ligand by hydroxyl ligand during electropolymerization of the monomer in aqueous solution. The fabricated electrode (poly([Cu(Bip)2OH]I)/GCE) was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The voltammetric behavior of CQ was examined using CV and square wave voltammetry (SWV). Compared to the bare GCE, poly(Bip)/GCE, and Cu/GCE, the current signal of CQ was significantly enhanced at poly([Cu(Bip)2OH]I)/GCE, which demonstrates excellent electrocatalytic behavior of poly([Cu(Bip)2OH]I)/GCE towards electrochemical oxidation of CQ. Under the optimum experimental conditions, the SWV current signal of poly([Cu(Bip)2OH]I)/GCE offered linearity on the concentration range of CQ between 0.5 and 250 μM with LOD and LOQ values of 4.22 ×10−2 and 1.4 × 10−1 μM, respectively. In the presence of possible interfering substances including glucose, paracetamol, adenine and guanine, the voltammetric determination of CQ was also considered, and their interventions were found to be insignificant, which evidenced the selectivity of the introduced electrode. The analytical application of the established sensor was successfully applied in the determination of CQ in pharmaceuticals, milk, serum, and urine samples. The detected amount of CQ in the tablet samples was in the range between 100.5 and 110.2% with RSD of 1.5 and 1.87%, respectively. The spiked recovery results in pharmaceuticals, milk, serum, and urine biological samples were in the range of 100.5 to 110.2%, 97.13 to 98.12, 103.7 to 103.6% and 95.50 to 97.05%, respectively. These results confirm that the developed method exhibits high applicability for electrochemical determination of CQ in various real samples.



中文翻译:

聚(双(2,2′-联吡啶)羟基碘化铜(II)修饰玻碳电极用于电化学测定药物和生物样品中的氯喹

采用电聚合法制备了一种新型电化学传感器——聚(双(2,2′-联吡啶)羟基铜(II)碘化物修饰玻碳电极(poly([Cu(Bip) 2 OH]I)/GCE) ,2'-联吡啶)氯化铜(II)碘化物([Cu(Bip) 2 Cl]I)在玻碳电极(GCE)上用于伏安法测定氯喹(CQ)。合成的络合物(双(2,2'-联吡啶) )氯铜(II)碘化物)使用UV-Vis进行表征,CHN元素分析,原子吸收光谱(AAS),电解电导率,熔点和傅里叶变换红外光谱(FT-IR)用于表征和确认合成所需的络合物(双(2,2'-联吡啶)碘化氯铜(II))。合成聚合物的紫外-可见光、傅立叶变换红外光谱和电化学数据支持单体在水溶液中电聚合过程中氯配体被羟基配体取代。通过循环伏安法(CV)和电化学阻抗谱(EIS)对制备的电极(聚([Cu(Bip)2 OH]I)/GCE)进行表征。使用 CV 和方波伏安法 (SWV) 检查 CQ 的伏安行为。与裸GCE、poly(Bip)/GCE和Cu/GCE相比,poly([Cu(Bip) 2 OH]I)/GCE上CQ的电流信号显着增强,这表明poly(Bip)/GCE具有优异的电催化性能。[Cu(Bip) 2 OH]I)/GCE 用于 CQ 的电化学氧化。在最佳实验条件下,poly([Cu(Bip) 2 OH]I)/GCE的SWV电流信号在CQ浓度范围0.5~250 μM之间呈现线性关系,LOD和LOQ值为4.22×10 -2和 1.4×分别为10 -1  μM。在存在可能的干扰物质(包括葡萄糖、扑热息痛、腺嘌呤和鸟嘌呤)的情况下,还考虑了伏安法测定CQ,发现它们的干扰微不足道,这证明了引入电极的选择性。所建立的传感器的分析应用已成功应用于药品、牛奶、血清和尿液样品中CQ的测定。片剂样品中 CQ 的检出量范围为 100.5% 至 110.2%,RSD 分别为 1.5% 和 1.87%。药物、牛奶、血清和尿液生物样品的加标回收率结果分别在100.5%至110.2%、97.13%至98.12%、103.7%至103.6%和95.50%至97.05%范围内。这些结果证实了所开发的方法对各种实际样品中 CQ 的电化学测定具有很高的适用性。

更新日期:2023-10-18
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