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Near Infrared and UV-Visible Spectroscopy Coupled with Chemometrics for the Characterization of Flours from Different Starch Origins 近红外和紫外-可见光谱法与化学计量学结合用于表征不同淀粉来源的面粉
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-22 DOI: 10.3390/chemosensors12010001
Samuele Pellacani, Marco Borsari, M. Cocchi, A. D’Alessandro, C. Durante, Giulia Farioli, L. Strani
This work tested near-infrared (NIR) and UV-visible (UV-Vis) spectroscopy coupled with chemometrics to characterize flours from different starch origins. In particular, eighteen starch-containing flours (e.g., type 00 flour, rye, barley, soybean, chestnut, potato, spelt, buckwheat, oat, millet, rice, durum wheat, amaranth, chickpea, sesame, corn, hemp and sunflower flours) were analyzed with a twofold objective: chemically characterizing the investigated flours and laying the groundwork for the development of a fast and suitable method that can identify the botanical source of starch in food. This could ensure ingredient traceability and aid in preventing/detecting food fraud. Untargeted approaches were used for this study, involving the simultaneous acquisition of a large amount of chemical information (UV-Vis on extracted starch and NIR signals on raw flours) coupled with chemometric techniques. UV-VIS spectra were acquired between 225 and 800 nm after sample pretreatment to extract starch. NIR spectra were acquired between 900 and 1700 nm using a poliSPEC NIRe portable instrument on the flours without any kind of pretreatments. An initial exploratory investigation was conducted using principal component analysis and cluster analysis, obtaining interesting preliminary information on patterns among the investigated flours. In particular, the UV-Vis model successfully discerned samples such as potato, chestnut, sunflower, durum wheat, sesame, buckwheat, rice, corn, spelt and 00-type flours. PCA model results obtained from the analysis of NIR spectra also provided comparable results with the UV-Vis model, particularly highlighting the differences observed between hemp and potato flours with soybean flour. Some similarities were identified between other flours, such as barley and millet, rye and oats, and chickpea and amaranth. Therefore, some flour samples underwent surface analysis via scanning electron microscope (SEM) using the Nova NanoSEM 450 to detect distinctive morphology.
这项工作测试了近红外(NIR)和紫外-可见(UV-Vis)光谱与化学计量学的结合,以表征不同淀粉来源的面粉。特别是对 18 种含淀粉的面粉(如 00 型面粉、黑麦、大麦、大豆、栗子、马铃薯、斯佩尔特小麦、荞麦、燕麦、小米、大米、硬质小麦、苋菜、鹰嘴豆、芝麻、玉米、大麻和向日葵面粉)进行了分析,目的有两个:对所研究的面粉进行化学特征描述,并为开发一种快速、合适的方法奠定基础,该方法可识别食品中淀粉的植物来源。这可以确保成分的可追溯性,并有助于预防/检测食品欺诈。本研究采用了非目标方法,包括同时获取大量化学信息(提取淀粉的紫外可见光谱和生面粉的近红外信号),并结合化学计量学技术。在样品预处理提取淀粉后,在 225 纳米和 800 纳米之间采集紫外可见光谱。使用 poliSPEC NIRe 便携式仪器对未经任何预处理的面粉采集了 900 至 1700 nm 的近红外光谱。利用主成分分析和聚类分析进行了初步的探索性研究,获得了关于所研究面粉之间模式的有趣的初步信息。特别是,紫外可见光谱模型成功地分辨出了马铃薯、栗子、向日葵、硬质小麦、芝麻、荞麦、大米、玉米、斯佩尔特小麦和 00 型面粉等样品。近红外光谱分析得出的 PCA 模型结果也与紫外可见光谱模型结果相当,尤其突出了大麻和马铃薯面粉与大豆面粉之间的差异。大麦和小米、黑麦和燕麦、鹰嘴豆和苋菜等其他面粉之间也有一些相似之处。因此,使用 Nova NanoSEM 450 通过扫描电子显微镜(SEM)对一些面粉样本进行了表面分析,以检测其独特的形态。
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引用次数: 0
Spectroscopy, a Tool for the Non-Destructive Sensory Analysis of Plant-Based Foods and Beverages: A Comprehensive Review 光谱学是对植物性食品和饮料进行非破坏性感官分析的工具:全面回顾
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-18 DOI: 10.3390/chemosensors11120579
T. Basile, D. Mallardi, M. Cardone
In recent years, there has been a significant rise in the popularity of plant-based products due to various reasons, such as ethical concerns, environmental sustainability, and health benefits. Sensory analysis is a powerful tool for evaluating the human appreciation of food and drink products. To link the sensory evaluation to the chemical and textural compositions, further quantitative analyses are required. Unfortunately, due to the destructive nature of sensory analysis techniques, quantitative evaluation can only be performed on samples that are different from those ingested. The quantitative knowledge of the analytical parameters of the exact sample ingested would be far more informative. Coupling non-destructive techniques, such as near-infrared (NIR) and hyperspectral imaging (HSI) spectroscopy, to sensory evaluation presents several advantages. The intact sample can be analyzed before ingestion, providing in a short amount of time matrices of quantitative data of several parameters at once. In this review, NIR and imaging-based techniques coupled with chemometrics based on artificial intelligence and machine learning for sensory evaluation are documented. To date, no review article covering the application of these non-destructive techniques to sensory analysis following a reproducible protocol has been published. This paper provides an objective and comprehensive overview of the current applications of spectroscopic and sensory analyses based on the state-of-the-art literature from 2000 to 2023.
近年来,由于道德关切、环境可持续性和健康益处等各种原因,植物基产品的受欢迎程度大幅上升。感官分析是评估人类对食品和饮料产品鉴赏力的有力工具。为了将感官评估与化学和质地成分联系起来,需要进一步进行定量分析。遗憾的是,由于感官分析技术的破坏性,定量评估只能在不同于摄入的样品上进行。对所摄入的确切样品的分析参数进行定量了解,信息量要大得多。将近红外(NIR)和高光谱成像(HSI)光谱等非破坏性技术与感官评估结合起来有几个优点。完整样品可在食用前进行分析,在短时间内同时提供多个参数的定量数据矩阵。本综述介绍了基于近红外和成像的技术,以及基于人工智能和机器学习的化学计量学在感官评估中的应用。迄今为止,还没有发表过一篇综述文章,介绍如何将这些非破坏性技术应用于按照可重复协议进行的感官分析。本文根据 2000 年至 2023 年的最新文献,客观、全面地概述了光谱和感官分析的当前应用。
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引用次数: 0
Rapid and Sensitive On-Site Detection of Fipronil in Foods Using Evanescent Wave Fluorescent Immunosensor 利用 Evanescent Wave 荧光免疫传感器快速灵敏地现场检测食品中的氟虫腈
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-17 DOI: 10.3390/chemosensors11120578
Yujing Li, Wenjuan Xu, Jingjing Liu, E. Zhang, Hejie Li, Yan Zhang, Jing Zhang, Chunsheng Li, Xiaoguang Zhang
Fipronil (FIP), a broad-spectrum phenylpyrazole insecticide, is highly toxic and threatens human health and ecological balance. Developing convenient, rapid, portable analytical technology for on-site and high-frequency testing of FIP is essential to reduce its damage. Herein, a monoclonal antibody (Clone F-3F6) against FIP, with high affinity and specificity, was produced using a novel immunogen, FIP-BSA, which was simply and directly synthesized by conjugating FIP with bovine serum albumin (BSA). Among the previously reported antibodies, F-3F6 acts more specifically against FIP. The FIP metabolites fipronil desulfinyl, fipronil sulfide, and fipronil sulfone showed lower cross-reactivity, and other pesticides were not recognized. To achieve high-frequency and on-site measurements of FIP, an evanescent wave fluorescence biosensor was built by integrating evanescent wave fluorescence technology, a functionalized fiber bioprobe, and a fluorescence-labeled F-3F6 antibody. The detection limit of FIP was 0.032 μg/L. The detection results of real milk and water samples showed that all the coefficients of variation were less than 10%, and the recovery ranged from 90 to 120%. The high reusability and stability of functionalized fiber bioprobe enables the accurate, cost-effective, high-frequency, and facile quantitative detection of FIP. This highly specific and reliable evanescent wave fluorescence biosensor will be well suited to the sensitive and high-frequency on-site analysis of only FIP in food.
氟虫腈(FIP)是一种广谱苯基吡唑类杀虫剂,具有剧毒,威胁人类健康和生态平衡。开发方便、快速、便携的分析技术,对氟虫腈进行现场高频检测,对减少其危害至关重要。本文利用一种新型免疫原 FIP-BSA 制备了一种针对 FIP 的单克隆抗体(克隆 F-3F6),该抗体具有高亲和力和特异性,FIP-BSA 是通过将 FIP 与牛血清白蛋白(BSA)结合而简单直接合成的。在之前报道的抗体中,F-3F6 对 FIP 的作用更具特异性。FIP 的代谢物氟虫腈脱亚硫酰基、氟虫腈硫醚和氟虫腈砜的交叉反应性较低,而其他农药则无法识别。为了实现对氟虫腈的高频和现场测量,研究人员集成了蒸发波荧光技术、功能化纤维生物探针和荧光标记的 F-3F6 抗体,建立了蒸发波荧光生物传感器。FIP 的检测限为 0.032 μg/L。对真实奶样和水样的检测结果表明,所有变异系数均小于 10%,回收率在 90% 至 120% 之间。功能化纤维生物探针的高重复使用性和稳定性使其能够准确、经济、高频、方便地定量检测 FIP。这种高特异性和高可靠性的蒸发波荧光生物传感器将非常适合于对食品中仅有的 FIP 进行灵敏和高频率的现场分析。
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引用次数: 0
Speciation of Iron Using Desferal via Simple pH Change and a Single Calibration Curve: High-Throughput Optical Sensor Based on 96-Well Plates and an Overhead Book Scanner as Detector 通过简单的 pH 值变化和单一的校准曲线利用脱盐法进行铁的种类分析:基于 96 孔板的高通量光学传感器和作为检测器的高架图书扫描仪
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-14 DOI: 10.3390/chemosensors11120577
Dimitrios Baltzis, Apostolia Tsiasioti, C. Zacharis, P. Tzanavaras
In the present study we report the development of an advantageous optical sensor for the speciation of Fe(III)/Fe(II). The sensor is based on the selective reaction of Fe(III) with a Desferal (Deferoxamine) reagent at pH = 2, while both Fe(III) and Fe(II) react with the reagent at pH = 5 using an acetate/glycine buffer. In this way, frequently used extra oxidation (H2O2) or reduction (ascorbic acid or hydroxylamine) steps are avoided. Both species can be determined in the range of 25 to 150 μM using a 96-well plate platform and the instrument-free detection of the colored complex with an overhead book scanner. The LOD is 4 μM, and an additional advantage is that a single calibration curve can be utilized for quantitation. The applicability of the sensor was demonstrated by analyzing commercially available pharmaceutical formulations for quality control purposes.
在本研究中,我们报告了一种用于铁(III)/铁(II)标样的优势光学传感器的开发情况。该传感器基于铁(III)在 pH = 2 时与 Desferal(去铁胺)试剂的选择性反应,而铁(III)和铁(II)在 pH = 5 时使用醋酸/甘氨酸缓冲液与试剂反应。这样就避免了经常使用的额外氧化(H2O2)或还原(抗坏血酸或羟胺)步骤。使用 96 孔板平台和高架扫描仪对有色复合物进行无仪器检测,可测定 25 至 150 μM 范围内的两种物质。检测限为 4 μM,另外一个优点是可以利用单一校准曲线进行定量。通过分析用于质量控制的市售药物制剂,证明了该传感器的适用性。
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引用次数: 0
Bioengineered Flagellin–TiO2 Nanoparticle-Based Modified Glassy Carbon Electrodes as a Highly Selective Platform for the Determination of Diclofenac Sodium 基于生物工程鞭毛菌素-TiO2 纳米粒子的改性玻璃碳电极作为高选择性平台用于测定双氯芬酸钠
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-07 DOI: 10.3390/chemosensors11120576
Juan Santiago Hidalgo, É. Tóth, H. Jankovics, C. I. Fort, G. Turdean, Etelka Tombácz, I. Galambos
This study describes the incorporation of bioengineered flagellin (4HIS) protein in conjunction with TiO2 anatase nanoparticles into a chitosan (Chit) polymeric matrix as a highly sensitive electrode modifier for the determination of diclofenac sodium (DS) in wastewater. Two types of electrodes were prepared using a simple drop-casting method. The inner structure of the obtained modified electrode was characterized by scanning electron microscopy (SEM) in combination with energy-dispersive X-ray spectroscopy and isothermal titration calorimetry (ITC). The electrochemical and electroanalytical parameters of DS oxidation at the nanostructured interface of the modified electrode were obtained via cyclic voltammetry and square-wave voltammetry. The analytical parameters for diclofenac electro-detection showed a 50% decrease in LOD and LOQ at Chit + TiO2 + 4HIS/GCE-modified electrode compared with the Chit + 4HIS/GCE-modified electrode. The obtained tools were successfully used for DS detection in drug tablets and wastewater samples. Thus, it was demonstrated that in the presence of a histidine-containing flagellin variant, the electrode has DS recognition capacity which increases in the presence of TiO2 nanoparticles, and both induce excellent performances of the prepared tools, either in synthetic solution or in real samples.
本研究描述了将生物工程鞭毛蛋白(4HIS)与二氧化钛锐钛酶纳米颗粒结合到壳聚糖(Chit)聚合物基质中,作为一种高灵敏度电极修饰剂,用于测定废水中的双氯芬酸钠(DS)。采用简单的滴铸法制备了两种电极。利用扫描电镜(SEM)、能量色散x射线能谱法和等温滴定量热法(ITC)对改性电极的内部结构进行了表征。通过循环伏安法和方波伏安法测定了改性电极纳米界面上DS氧化的电化学和电分析参数。双氯芬酸电检测分析参数显示,Chit + TiO2 + 4HIS/ gce修饰电极的LOD和LOQ比Chit + 4HIS/ gce修饰电极降低了50%。该工具可用于药物片剂和废水样品的DS检测。因此,实验证明,在含有组氨酸的鞭毛蛋白变体存在的情况下,电极具有DS识别能力,并且在TiO2纳米颗粒存在的情况下,电极具有DS识别能力,并且无论是在合成溶液中还是在实际样品中,都能诱导制备的工具具有优异的性能。
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引用次数: 0
Electrochemical Sensing of Vitamin D3: A Comparative Use of Glassy Carbon and Unmodified Screen-Printed Carbon Electrodes 维生素 D3 的电化学传感:玻璃碳电极与未改性丝网印刷碳电极的比较使用
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-06 DOI: 10.3390/chemosensors11120575
Fátima Daniela Gonçalves, José António Rodrigues, R. M. Ramos
This work presents the electrochemical determination of cholecalciferol (Vitamin D3) in water-organic mixtures using a glassy carbon electrode (GCE) and commercial screen-printed carbon electrodes (SPCEs). The electrocatalytic behavior of Vitamin D3 on the surface of the working electrode produced a well-defined oxidation peak at +0.95 V (vs. Ag|AgCl, 3.0 mol L−1) and +0.7 V (vs. Ag-SPCE pseudo-reference electrode) for the GCE and SPCE, respectively, in 0.1 M LiClO4 prepared in 50% ethanol. The nature of the organic solvent needed for the solubilization of Vitamin D3 was evaluated, together with the concentration of the supporting electrolyte, the ratio of the water-organic mixture, the voltametric parameters for the cyclic voltammetry (CV), and square-wave voltammetry (SWV) analyses. Under the optimized conditions, a linear correlation between the anodic peak current and the concentration of Vitamin D3 was obtained over the range of 0.47 to 123 µmol L−1 and 59.4 to 1651 µmol L−1 for the GCE and SPCE, respectively. The determined limits of detection (LOD) were 0.17 (GCE) and 19.4 µmol L−1 (SPCE). The methodology was successfully applied to commercial supplement tablets of Vitamin D3. Additionally, this work shows the possibility of using non-modified GCE and SPCE for routine analysis of Vitamin D3.
本文介绍了利用玻璃碳电极(GCE)和商业丝网印刷碳电极(SPCEs)电化学测定水-有机混合物中胆钙化醇(维生素D3)的方法。在50%乙醇中制备的0.1 M LiClO4中,维生素D3在工作电极表面的电催化行为产生了明确的氧化峰,分别为+0.95 V (vs. Ag|AgCl, 3.0 mol L−1)和+0.7 V (vs. Ag-SPCE伪参比电极)。考察了维生素D3增溶所需的有机溶剂的性质,以及支持电解质的浓度、水-有机混合物的比例、循环伏安法(CV)和方波伏安法(SWV)分析的伏安参数。在优化条件下,GCE和SPCE的阳极峰电流与维生素D3浓度分别在0.47 ~ 123µmol L−1和59.4 ~ 1651µmol L−1范围内呈线性相关。测定的检出限(LOD)分别为0.17 (GCE)和19.4µmol L−1 (SPCE)。该方法已成功地应用于商业维生素D3补充剂片。此外,这项工作显示了使用未修饰的GCE和SPCE进行维生素D3常规分析的可能性。
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引用次数: 0
Laser-Scribed Pencil Lead Electrodes for Amperometric Quantification of Indapamide 用于吲达帕胺安培定量的激光刻蚀铅笔芯电极
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-05 DOI: 10.3390/chemosensors11120574
Thawan G. Oliveira, Irlan S. Lima, Wilson A. Ameku, J. Gonçalves, Rodrigo S. Souza, Henrique E. Toma, L. Angnes
Laser engraving is a convenient, fast, one-step, and environmentally friendly technique used to produce more conductive surfaces by local pyrolysis. The laser’s thermal treatment can also remove non-conductive materials from the electrode surfaces and improve electrochemical performance. The improvement was assessed by electrochemical tools such as cyclic voltammograms and electrochemical impedance spectroscopy using [Fe(CN)6]3−/4− and dopamine as redox probes. The electrochemical results observed showed that a treated surface showed an improvement in electron transfer and less resistance to charge transfer. To optimize the electrode performance, it was necessary to search for the most favorable graphite mines and optimize the parameters of the laser machine (laser power, scan rate, and output distance). The resultant material was adequately characterized by Raman spectroscopy and scanning electron microscopy (SEM), where an irregular surface composed of crystalline graphite particles was noticed. Furthermore, as a proof-of-concept, it was applied to detect indapamide (IND) in synthetic urine by flow injection analysis (FIA), a diuretic drug often used by athletes to alter urine composition to hide forbidden substance consumption in doping tests.
激光雕刻是一种方便、快速、一步、环保的技术,用于通过局部热解产生更多的导电表面。激光热处理还可以去除电极表面的非导电材料,提高电化学性能。使用[Fe(CN)6]3−/4−和多巴胺作为氧化还原探针,通过循环伏安图和电化学阻抗谱等电化学工具评估了这种改善。电化学结果表明,处理后的表面电子转移能力增强,电荷转移阻力减小。为了优化电极性能,需要寻找最有利的石墨矿,优化激光器的参数(激光功率、扫描速率和输出距离)。通过拉曼光谱和扫描电子显微镜(SEM)对所得材料进行了充分的表征,其中注意到由结晶石墨颗粒组成的不规则表面。此外,作为概念验证,它被应用于通过流动注射分析(FIA)检测合成尿中的吲达帕胺(IND),这是一种利尿剂,运动员经常在兴奋剂测试中使用它来改变尿液成分,以掩盖违禁物质的摄入。
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引用次数: 0
An Electrochemical Immunosensor with PEDOT: PSS/MWCNTs-COOH Nanocomposites as a Modified Working Electrode Material for Detecting Tau-441 用 PEDOT:以 PEDOT: PSS/MWCNTs-COOH 纳米复合材料为改良工作电极材料检测 Tau-441 的电化学免疫传感器
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-04 DOI: 10.3390/chemosensors11120573
Hanwen Ren, Xiansu Liu, Shanshan Wei, F. Zhao, Zhencheng Chen, H. Xiao
The progression of Alzheimer’s disease (AD) is positively correlated with the phosphorylation damage of Tau-441 protein, which is the marker with the most potential for the early detection of AD. The low content of Tau-441 in human serum is a major difficulty for the realization of content detection. Herein, we prepared an electrochemical immunosensor modified with Poly(3,4-ethylene-dioxythiophene)-poly (styrene sulfonate) (PEDOT: PSS)/Carboxylated multi-walled carbon nanotube (MWCNTs-COOH) nanocomposites based on electrochemical immunoassay technology for the low-concentration detection of Tau-441. The immunosensor based on the nanocomposite can take advantage of the characteristics of conductive polymers to achieve electrical signal amplification and use MWCNTs-COOH to increase the contact area of the active site and bond with the Tau-441 antibodies on the electrode. The physicochemical and electrical properties of PEDOT: PSS/MWCNTs-COOH were studied by in situ characterization techniques and electrochemical characterization methods, indicating that the immunosensor has high selectivity and sensitivity to the Tau-441 immune reaction. Under optimized optimal conditions, the electrochemical immunosensor detected a range of concentrations of Tau-441 to obtain a low detection of limit (0.0074 ng mL−1) and demonstrated good detection performance through actual human serum sample testing experiments. Therefore, the study provides an effective reference value for the early diagnosis of AD.
Tau-441蛋白磷酸化损伤与阿尔茨海默病(AD)的进展呈正相关,是最有可能早期发现AD的标志物。人血清中Tau-441含量低是实现其含量检测的主要困难。本文基于电化学免疫分析技术,制备了以聚(3,4-乙烯-二氧噻吩)-聚苯乙烯磺酸盐(PEDOT: PSS)/羧化多壁碳纳米管(MWCNTs-COOH)纳米复合材料修饰的电化学免疫传感器,用于低浓度检测Tau-441。基于纳米复合材料的免疫传感器可以利用导电聚合物的特性实现电信号放大,并利用MWCNTs-COOH增加活性位点的接触面积,与电极上的Tau-441抗体结合。通过原位表征技术和电化学表征方法研究了PEDOT: PSS/MWCNTs-COOH的物理化学和电学性质,表明该免疫传感器对Tau-441免疫反应具有较高的选择性和敏感性。在优化后的最优条件下,电化学免疫传感器对一定浓度范围内的Tau-441进行检测,获得了较低的检出限(0.0074 ng mL−1),并通过实际人血清样品检测实验证明了良好的检测性能。因此,本研究为AD的早期诊断提供了有效的参考价值。
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引用次数: 0
Correction: Mokrushin et al. Chemoresistive Properties of V2CTx MXene and the V2CTx/V3O7 Nanocomposite Based on It. Chemosensors 2023, 11, 142 更正:Mokrushin 等人,V2CTx MXene 及其 V2CTx/V3O7 纳米复合材料的化学电阻特性。化学传感器 2023,11,142
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-04 DOI: 10.3390/chemosensors11120572
A. S. Mokrushin, I. A. Nagornov, A. Averin, T. Simonenko, N. Simonenko, E. Simonenko, N. T. Kuznetsov
In the original publication, there was a mistake in “Figure 5 [...]
在原始出版物中,“图5[…]”中有一个错误。
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引用次数: 0
A Selective Fluorescent Optode for Lead(II) Based on the Dansylamidopropyl Pendant Arm Derivative of 1,4-dioxa-7,13-dithia-10-Azacyclopentadecane ([15]aneNS2O2) 基于 1,4-二氧杂-7,13-二硫杂-10-氮杂环十五烷([15]aneNS2O2)的丹酰胺丙基悬臂衍生物的铅(II)选择性荧光光电管
IF 4.2 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-01 DOI: 10.3390/chemosensors11120571
Mojtaba Shamsipur, Moslem Mohammadi, M. Arca, A. Garau, V. Lippolis, Ali Barati
In this study, a novel highly sensitive and selective fluorescent optode membrane aimed at the determination of Pb(II) ion is proposed by incorporating N-(3-(1,4-dioxa-7,13-dithia-10-azacyclopentadecan-10-yl)propyl)-5-(dimethylamino)naphthalene-1-sulfonamide (L) as fluoroionophore in polyvinyl chloride (PVC) containing 2-nitrophenyl octylether (NPOE) as a plasticizer. In addition to high stability and reproducibility, the proposed optosensor showed a unique selectivity toward Pb(II) ion, with a wide linear range of molar concentrations (1.0 × 10−9–1.0 × 10−3 M) and a low detection limit of 7.5 × 10−10 M in solution at pH 5.0. The formation constants of the Pb(II) complexes with the fluoroionophore were evaluated by fitting the fluorescence data with a nonlinear least-squares curve-fitting program, and further information about the structures of the complexes were evaluated based on hybrid-DFT calculations. The optosensor exhibited a fast response time of less than three min, being easily regenerated by exposure to a solution of dithiothreitol. The sensor was applied to the determination of Pb(II) in real samples (canned tuna fish), and it provided satisfactory results comparable to those obtained via atomic absorption spectrometry (AAS).
本研究以N-(3-(1,4-二氧杂甲-7,13-二硫-10-氮杂环戊烷-10-基)丙基)-5-(二甲氨基)萘-1-磺酰胺(L)为荧光离子载体,在含2-硝基苯辛基醚(NPOE)的聚氯乙烯(PVC)中作为增塑剂,制备了一种用于测定铅(II)离子的高灵敏度、高选择性荧光光电膜。除了高稳定性和重复性外,该光传感器对Pb(II)离子具有独特的选择性,其摩尔浓度线性范围宽(1.0 × 10−9 ~ 1.0 × 10−3 M),在pH 5.0的溶液中检测限低至7.5 × 10−10 M。利用非线性最小二乘曲线拟合程序对荧光数据进行拟合,确定了含氟离子载体的Pb(II)配合物的形成常数,并基于混合dft计算进一步确定了配合物的结构信息。该光传感器具有小于3 min的快速响应时间,并且易于暴露于二硫苏糖醇溶液中再生。将该传感器应用于实际样品(金枪鱼罐头)中Pb(II)的测定,结果与原子吸收光谱法(AAS)相当。
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Chemosensors
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