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采用还原氧化石墨烯传感器的吸附溶出伏安法测定牛奶样品中氯霉素残留量

Adsorptive stripping voltammetric determination of chloramphenicol residues in milk samples using reduced graphene oxide sensor.

机构信息

NUPIS (Núcleo de Pesquisa em Instrumentação e Separações Analíticas), Departamento de Química, Instituto de Ciências Exatas, Universidade Federal de Juiz de Fora, Juiz de Fora, MG, 36036-900, Brazil.

Instituto de Química, Universidade Federal de Uberlândia, Uberlândia, MG, 38400-902, Brazil.

出版信息

Anal Methods. 2021 Dec 9;13(47):5711-5718. doi: 10.1039/d1ay01756j.

Abstract

In this paper, the electrochemical response of chloramphenicol (CHL) was investigated on a bare glassy carbon electrode (GCE) and after modification with reduced graphene oxide (GCE/rGO). Preliminary studies by cyclic voltammetry demonstrated an adsorption-controlled mass transport regime of CHL species and a pH-dependent behavior on both electrode surfaces. An adsorptive stripping differential pulse voltammetry (AdSDPV) method was proposed and under optimized instrumental conditions, a comparison of the analytical characteristics of both sensors was performed. The GCE/rGO sensor showed an increase in sensitivity (10-fold), and an anticipation of the reduction potential (200 mV), compared to the bare electrode, due to the adsorptive character (pre-concentration of the CHL species) and the electrocatalytic effect of the nanomaterial. The method was applied to skimmed and whole milk samples, which were simply diluted (50-fold) in supporting electrolyte. The results by AdSDPV using GCE/rGO showed adequate detectability (0.22 μmol L), good precision with a 6% relative standard deviation (RSD) and satisfactory recovery ranging from 93 to 108%. The obtained results were statistically similar (95% confidence level) with those performed through ultra-fast liquid chromatography (UFLC). Furthermore, the sensor showed an improvement in the analytical performance for CHL detection, when compared to other sensors reported in the literature. Therefore, the developed method is reliable and promising for implementation in monitoring CHL residues in milk samples.

摘要

本文研究了在裸玻碳电极(GCE)和还原氧化石墨烯修饰的玻碳电极(GCE/rGO)上氯霉素(CHL)的电化学响应。循环伏安法的初步研究表明,CHL 物种在两种电极表面均存在吸附控制的质量传输和 pH 值依赖性。提出了一种吸附溶出差分脉冲伏安法(AdSDPV)方法,并在优化的仪器条件下,比较了两种传感器的分析特性。与裸电极相比,GCE/rGO 传感器的灵敏度提高了 10 倍,还原电位提前了 200 mV,这是由于纳米材料的吸附特性(CHL 物种的预浓缩)和电催化作用。该方法应用于脱脂和全脂牛奶样品,只需在支持电解质中简单稀释(50 倍)。使用 GCE/rGO 的 AdSDPV 方法的结果显示出足够的检测能力(0.22 μmol L),6%的相对标准偏差(RSD)具有良好的精密度,回收率从 93%到 108%令人满意。获得的结果与通过超快速液相色谱(UFLC)进行的结果在统计学上相似(置信水平为 95%)。此外,与文献中报道的其他传感器相比,该传感器在 CHL 检测的分析性能方面有所提高。因此,该方法可靠且有望用于监测牛奶样品中的 CHL 残留。

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