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Using magnetic nanoparticles/MIP-based electrochemical sensor for quantification of tetracycline in milk samples
Journal of Electroanalytical Chemistry ( IF 4.5 ) Pub Date : 2021-09-17 , DOI: 10.1016/j.jelechem.2021.115713
Shakeel Zeb 1, 2 , Ademar Wong 1, 2 , Sabir Khan 1, 3 , Sajjad Hussain 4 , Maria D.P.T. Sotomayor 1, 2
Affiliation  

This paper reports the development of a biomimetic sensor and its application for the determination of tetracycline antibiotics. Tetracycline is an extremely vital antibiotic usually used for the treatment of people and livestock with bacterial disorder and respiratory issues. This antibiotic is widely used in poultry farms for the prevention of bacterial infection and the treatment of advanced bacterial growth. The sensor was constructed using magnetic nanoparticles (mag) and molecularly imprinted polymer (MIP). Based on the application of the co-precipitation approach, FeCl3·6H2O and FeCl2·4H2O salts were used to obtain core@shell magnetic nanoparticles. Prior to the synthesis of the selective MIP material, the density functional theory (DFT) was used to select the best functional monomer for the analyte investigated. After choosing the best monomer, the modified magnetic nanoparticles were used for the synthesis of the MIP in order to enhance the detection capability of the electrochemical sensor. The imprinted polymer was synthesized using optimized amounts of acrylic acid (functional monomer), ethylene–glycol-dimethacrylate (cross-linker), and 2,2 azobisisobutyronitrile (radical initiator). The control material – denoted by mag-NIP (magnetic non-molecularly imprinted polymer), which was used for comparison purposes, was synthesized based on the same procedure applied for the synthesis of the MIP but in the absence of the analyte (tetracycline). The analysis of surface morphology and the identification of the functional groups used in the synthesized magnetic materials were performed by fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), and high-resolution electron microscopy. The detection of tetracycline was performed under optimized conditions using square wave voltammetry, 15 mg of mag-MIP (on carbon paste), and 80 s of pre-concentration. Through the application of this analysis, well-defined peaks ranging from 0.5 to 1.0 V vs. Ag/AgCl (KClsat) were obtained. Analytical curves were constructed using the second peak at 0.83 V, and the following results were obtained: linear range of 5.0 × 10−7 to 4.0 × 10−5 mol L−1 (R2 of 0.9993), limit of detection (LOD) of 1.5 × 10−7 mol L−1 and repeatability of 2.82% (in terms of relative standard deviation) for n = 10. The results obtained from the analysis of selectivity demonstrated that the proposed electrochemical sensor is highly efficient for tetracycline determination. The sensor was successfully applied in commercial and raw milk samples for tetracycline detection, and recovery rates ranging from 93 − 103% were obtained. The results obtained show that the proposed electrochemical technique is suitable for application toward the determination of tetracycline.



中文翻译:

使用磁性纳米粒子/基于 MIP 的电化学传感器定量牛奶样品中的四环素

本文报道了仿生传感器的开发及其在四环素类抗生素检测中的应用。四环素是一种极其重要的抗生素,通常用于治疗患有细菌性疾病和呼吸系统疾病的人和牲畜。这种抗生素广泛用于家禽养殖场,用于预防细菌感染和治疗晚期细菌生长。该传感器使用磁性纳米粒子 (mag) 和分子印迹聚合物 (MIP) 构建。基于共沉淀法的应用,FeCl 3 ·6H 2 O和FeCl 2 ·4H 2O盐用于获得核@壳磁性纳米粒子。在合成选择性 MIP 材料之前,使用密度泛函理论 (DFT) 为所研究的分析物选择最佳功能单体。在选择最佳单体后,将修饰的磁性纳米粒子用于合成 MIP,以提高电化学传感器的检测能力。使用优化量的丙烯酸(功能单体)、乙二醇二甲基丙烯酸酯(交联剂)和 2,2 偶氮二异丁腈(自由基引发剂)合成印迹聚合物。对照材料——由 mag-NIP(磁性非分子印迹聚合物)表示,用于比较目的,基于用于合成 MIP 的相同程序合成,但不存在分析物(四环素)。通过傅里叶变换红外光谱 (FTIR)、场发射扫描电子显微镜 (FESEM) 和高分辨率电子显微镜进行表面形貌分析和合成磁性材料中使用的官能团的鉴定。四环素的检测在优化条件下使用方波伏安法、15 mg mag-MIP(在碳糊上)和 80 s 的预浓缩进行。通过该分析的应用,范围从 0.5 到 1.0 V 的明确峰 通过傅里叶变换红外光谱 (FTIR)、场发射扫描电子显微镜 (FESEM) 和高分辨率电子显微镜进行表面形貌分析和合成磁性材料中使用的官能团的鉴定。四环素的检测在优化条件下使用方波伏安法、15 mg mag-MIP(在碳糊上)和 80 s 的预浓缩进行。通过该分析的应用,范围从 0.5 到 1.0 V 的明确峰 通过傅里叶变换红外光谱 (FTIR)、场发射扫描电子显微镜 (FESEM) 和高分辨率电子显微镜进行表面形貌分析和合成磁性材料中使用的官能团的鉴定。四环素的检测在优化条件下使用方波伏安法、15 mg mag-MIP(在碳糊上)和 80 s 的预浓缩进行。通过该分析的应用,范围从 0.5 到 1.0 V 的明确峰. 获得Ag/AgCl (KCl sat )。使用 0.83 V 处的第二个峰构建分析曲线,获得以下结果:线性范围为 5.0 × 10 -7至 4.0 × 10 -5 mol L -1 (R 2为 0.9993),检测限 (LOD) 1.5 × 10 -7 mol L -1对于 n = 10,重复性为 2.82%(相对标准偏差而言)。从选择性分析中获得的结果表明,所提出的电化学传感器对于四环素测定非常有效。该传感器成功应用于商业和原料奶样品中进行四环素检测,回收率范围为 93 - 103%。所得结果表明所提出的电化学技术适用于测定四环素。

更新日期:2021-09-22
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