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基于分子印迹聚吡咯的磺胺二甲氧嘧啶电化学传感器:印迹参数研究。

Electrochemical sensor for sulfadimethoxine based on molecularly imprinted polypyrrole: study of imprinting parameters.

机构信息

Dipartimento di Scienze e Tecnologie Biologiche e Ambientali (Di.S.Te.B.A.), Università del Salento, via Monteroni, 73100 Lecce, Italy.

NanoInnovation Laboratory, Elettra Sincrotrone Trieste S.C.p.A., S.S.14 Km 163.5, 34149 Basovizza, Trieste, Italy.

出版信息

Biosens Bioelectron. 2015 Jan 15;63:240-247. doi: 10.1016/j.bios.2014.07.045. Epub 2014 Jul 25.

Abstract

The present work describes the development of a simple and cost-effective electrochemical sensor for sulfadimethoxine (SDM) based on molecularly imprinted overoxidized polypyrrole (PPy). An all electrochemical approach is used for sensor fabrication and application consisting in molecularly imprinted polymer (MIP) galvanostatic deposition on a gold electrode and its overoxidation under different experimental conditions and in SDM amperometric detection. Several parameters influencing the imprinting effect are critically discussed and evaluated. A key role of the electrolyte used in electropolymerization (tetrabuthylammonium perchlorate and lithium perchlorate) has emerged demonstrating its effect on sensing performances of imprinted PPy and, related to this, on its morphology, as highlighted by atomic force microscopy (AFM). The effect of different overoxidation conditions in removing template is evaluated by analyzing MIP films before and after the treatment by X-ray photoelectron spectroscopy (XPS) also evidencing the correlation between MIP chemical structure and its rebinding ability. MIP-template interaction is verified also by Fourier Transform Infrared (FT-IR) spectroscopy. Under the selected optimal conditions, MIP sensor shows a linear range from 0.15 to 3.7 mM SDM, a limit of detection of 70 μM, a highly reproducible response (RSD 4.2%) and a good selectivity in the presence of structurally related molecules. SDM was determined in milk samples spiked at two concentration levels: 0.2 mM and 0.4 mM obtaining a satisfactory recovery of (97±3)% and (96±8)%, respectively.

摘要

本工作描述了一种基于过氧氧化聚吡咯(PPy)的磺胺二甲氧嘧啶(SDM)分子印迹电化学传感器的研制。采用全电化学方法进行传感器的制备和应用,包括在金电极上电聚合分子印迹聚合物(MIP)和在不同实验条件下对其进行过氧化以及在 SDM 的安培检测中进行过氧化。对影响印迹效果的几个参数进行了深入讨论和评价。聚合中使用的电解质(高氯酸四丁基铵和高氯酸锂)的关键作用已经显现出来,证明了它对印迹 PPy 的传感性能的影响,以及与之相关的,对其形态的影响,原子力显微镜(AFM)对此进行了强调。通过分析处理前后的 MIP 薄膜,评估了不同过氧化条件对模板去除的影响,X 射线光电子能谱(XPS)也证明了 MIP 化学结构与其再结合能力之间的相关性。傅里叶变换红外(FT-IR)光谱也验证了 MIP-模板相互作用。在选择的最佳条件下,MIP 传感器在 0.15 至 3.7 mM SDM 的范围内呈现线性范围,检测限为 70 μM,具有高度重现性的响应(RSD 为 4.2%),并且在存在结构相关分子的情况下具有良好的选择性。在两个浓度水平(0.2 mM 和 0.4 mM)下对牛奶样品进行了 SDM 的测定,分别获得了 97±3%和 96±8%的令人满意的回收率。

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