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Simultaneous determination of pindolol, acebutolol and metoprolol in waters by differential-pulse voltammetry using an efficient sensor based on carbon paste electrode modified with amino-functionalized mesostructured silica
Sensors and Actuators B: Chemical ( IF 8.4 ) Pub Date : 2018-12-12 , DOI: 10.1016/j.snb.2018.12.058
Mariana Silva , Sonia Morante-Zarcero , Damián Pérez-Quintanilla , Isabel Sierra

In this work, hexagonal mesoporous silica (HMS) and amino-functionalized HMS (HMS-NH2) were prepared and incorporated into carbon paste electrodes (CPEs) to obtain electrochemical sensors for pindolol (Pin), acebutolol (Ace) and metoprolol (Met) determination in waters by voltammetric techniques. The materials were characterized and they showed high specific surface area, large pore volume and a quasi-spherical morphology. Firstly, the electrochemical behaviour of the modified CPEs was studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Then, the dependence of the current intensity with the electrolyte support (type and pH) and the accumulation time was investigated to optimize the experimental conditions for simultaneous β-blockers determination by DPV. Results showed that the sensor modified with functionalized silica (NH2-HMS-CPE) exhibited strong adsorption activity, showing three well-defined peaks in the differential pulse voltammograms, that appeared at about +0.85 V (Pin), +1.11 V (Ace) and +1.45 V (Met). This fact can be attributed to the high surface area of the material, with a 3 D wormhole-like channel structure that favoured excellent pore accessibility, and the synergistic effect produced by the grafted amino groups producing hydrogen bond interactions with the oxygen atoms of the target β-blockers. The prepared sensor exhibits good reproducibility, wide linear ranges and very low detection limits (0.1, 0.046 and 0.23 μmol L−1 for Pin, Ace and Met, respectively). Moreover, the NH2-HMS-CPE was successfully applied for the simultaneous determination of Pin, Ace and Met in tap, mineral, river and sewage effluent waters with simple sample treatment (recoveries 97–112%).



中文翻译:

基于氨基官能化介孔结构二氧化硅修饰的碳糊电极的高效传感器,通过差分脉冲伏安法同时测定水中的潘多洛尔,醋丁酚和美托洛尔

在这项工作中,六角形介孔二氧化硅(HMS)和氨基官能化HMS(HMS-NH 2制备)并结合到碳糊电极(CPE)中,以通过伏安法在水中测定潘多洛尔(Pin),醋丁洛尔(Ace)和美托洛尔(Met)的电化学传感器。对材料进行了表征,它们显示出高的比表面积,大的孔体积和准球形形态。首先,通过循环伏安法(CV)和差示脉冲伏安法(DPV)研究了改性CPE的电化学行为。然后,研究了电流强度与电解质载体(类型和pH)和累积时间的关系,以优化通过DPV同时测定β受体阻滞剂的实验条件。结果表明,传感器用功能化二氧化硅(NH 2-HMS-CPE)表现出很强的吸附活性,在差分脉冲伏安图中显示了三个明确定义的峰,分别出现在+0.85 V(Pin),+ 1.11 V(Ace)和+1.45 V(Met)处。这一事实可归因于材料的高表面积,具有3D虫洞状通道结构,有利于出色的孔可及性,并且由接枝的氨基产生的协同效应产生了与目标氧原子的氢键相互作用β受体阻滞剂。所制备的传感器表现出良好的可重复性,宽线性范围和非常低的检测限(Pin,Ace和Met分别为0.1、0.046和0.23μmolL -1)。此外,NH 2-HMS-CPE可以通过简单的样品处理成功地同时测定自来水,矿泉水,河流和污水中的Pin,Ace和Met(回收率97-112%)。

更新日期:2018-12-12
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