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裸石墨-聚氨酯复合电极在未经修饰和经石墨烯及碳纳米管修饰后的电化学测定艾司西酞普兰中的比较性能。

Comparative performances of a bare graphite-polyurethane composite electrode unmodified and modified with graphene and carbon nanotubes in the electrochemical determination of escitalopram.

机构信息

Instituto de Química de São Carlos, Universidade de São Paulo, 13566-590 São Carlos, SP, Brazil.

Instituto de Química de São Carlos, Universidade de São Paulo, 13566-590 São Carlos, SP, Brazil.

出版信息

Talanta. 2018 Feb 1;178:1024-1032. doi: 10.1016/j.talanta.2017.08.094. Epub 2017 Sep 1.

Abstract

A bare composite graphite-polyurethane electrode (EGPU) and two other modified with graphene (EGPU-GR) and functionalized multi-walled carbon nanotubes (EGPU-CNTs) were prepared and compared regarding their voltammetric response to escitalopran (EST). The modifiers were characterized by Raman spectroscopy and the resulting electrode materials by contact angle measurements with a hydrophilicity character in the ascending order for the composites: GPU > GPU-GR > GPU-CNTs and scanning electron microscopy (SEM). The electroactive areas of the EGPU, EGPU-GR, and EGPU-CNTs were 0.065, 0.080, and 0.092cm, respectively, calculated from the chronocoulometry using K[Fe(CN)] as a probe and the Cottrell equation. The cyclic voltammograms obtained for EST indicated irreversible electrochemical behavior, with an anodic peak at ca. +0.80V (νs. SCE). These measurements were carried out with the three electrodes, and comparison of the analytical responses led to the EGPU-GR electrode being selected for use in the subsequent experiments. Under optimal conditions, square wave and differential pulse voltammetry at EGPU-GR presented linear dynamic ranges between 1.5 × 10 and 1.2 × 10mol L, with a detection limit of 2.5 × 10molL (SWV) and 1.5 × 10 and 1.2 × 10molL, with a detection limit of 3.2 × 10molL (DPV) for EST. The proposed method was applied for the quantification of EST in synthetic urine and cerebrospinal fluid samples, offering advantages including simplicity of fabrication, no requirement for analyte preconcentration and surface renewal, fast response, and selectivity.

摘要

一种裸露的复合石墨-聚氨酯电极(EGPU)和另外两种经过石墨烯修饰的电极(EGPU-GR)和功能化多壁碳纳米管修饰的电极(EGPU-CNTs)被制备出来,并就它们对艾司西酞普兰(EST)的伏安响应进行了比较。修饰剂通过拉曼光谱进行了表征,所得电极材料通过接触角测量进行了表征,亲水性顺序为复合材料:GPU > GPU-GR > GPU-CNTs 和扫描电子显微镜(SEM)。使用 K[Fe(CN)]作为探针和 Cottrell 方程通过计时库仑法计算,得到 EGPU、EGPU-GR 和 EGPU-CNTs 的电化学活性面积分别为 0.065、0.080 和 0.092cm。EST 的循环伏安图表明为不可逆电化学行为,在约 +0.80V(vs. SCE)处有一个阳极峰。这些测量是在三电极系统中进行的,对分析响应的比较导致选择 EGPU-GR 电极用于后续实验。在最佳条件下,EGPU-GR 的方波和差分脉冲伏安法在 1.5 × 10 和 1.2 × 10mol L 之间呈现线性动态范围,检测限为 2.5 × 10molL(SWV)和 1.5 × 10 和 1.2 × 10molL,检测限为 3.2 × 10molL(DPV)用于 EST。该方法被应用于合成尿液和脑脊液样本中 EST 的定量,具有制造简单、无需对分析物进行预浓缩和表面更新、快速响应和选择性等优点。

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