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14 pages, 2360 KiB

Open AccessArticle

Bioengineered Flagellin–TiO₂ Nanoparticle-Based Modified Glassy Carbon Electrodes as a Highly Selective Platform for the Determination of Diclofenac Sodium

by Juan Santiago Hidalgo, Éva Tóth, Hajnalka Jankovics, Carmen Ioana Fort, Graziella Liana Turdean, Etelka Tombacz and Ildiko Galambos

Chemosensors 2023, 11(12), 576; https://doi.org/10.3390/chemosensors11120576 - 7 Dec 2023

Viewed by 1628

Abstract

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 [...] Read more.

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. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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12 pages, 2352 KiB

Open AccessArticle

Disposable Stochastic Platform for the Simultaneous Determination of Calcipotriol and Betamethasone in Pharmaceutical and Surface Water Samples

by Bianca-Maria Tuchiu, Raluca-Ioana Stefan-van Staden, Jacobus (Koos) Frederick van Staden and Hassan Y. Aboul-Enein

Chemosensors 2023, 11(8), 446; https://doi.org/10.3390/chemosensors11080446 - 10 Aug 2023

Viewed by 978

Abstract

A disposable stochastic platform based on calix [6]arene modified multi-walled carbon nanotubes-gold nanoparticles screen-printed electrode has been developed for the simultaneous determination of calcipotriol and betamethasone. For both analytes, very wide linear concentration ranges and extremely low limits of quantification (LOQ) were obtained: [...] Read more.

A disposable stochastic platform based on calix [6]arene modified multi-walled carbon nanotubes-gold nanoparticles screen-printed electrode has been developed for the simultaneous determination of calcipotriol and betamethasone. For both analytes, very wide linear concentration ranges and extremely low limits of quantification (LOQ) were obtained: from 1.0 × 10⁻¹⁵ to 1.0 × 10⁻³ mol L⁻¹ and with a 1.0 × 10⁻¹⁵ mol L⁻¹ LOQ for calcipotriol, and from 1.0 × 10⁻¹⁶ to 1.0 × 10⁻² mol L⁻¹ with a 1.0 × 10⁻¹⁶ mol L⁻¹ LOQ for betamethasone. The applicability of the sensing platform was successfully tested in commercially available topical pharmaceutical gel and surface water samples, obtaining recovery values ranging from 99.10 to 99.99% and relative standard deviation values under 0.05%. The obtained results render the proposed platform a viable, robust, selective, and sensitive tool that can be employed for the determination of the analytes in on-site routine quality control of pharmaceuticals and water quality monitoring. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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11 pages, 3838 KiB

Open AccessArticle

Enantioanalysis of Leucine in Whole Blood Samples Using Enantioselective, Stochastic Sensors

by Raluca-Ioana Stefan-van Staden and Oana-Raluca Musat

Chemosensors 2023, 11(5), 259; https://doi.org/10.3390/chemosensors11050259 - 22 Apr 2023

Cited by 1 | Viewed by 1183

Abstract

Enantioanalysis of amino acids became a key factor in the metabolomics of cancer. As a screening method, it can provide information about the state of health of patients. The main purpose of the study is to develop a highly reliable enantioanalysis method for [...] Read more.

Enantioanalysis of amino acids became a key factor in the metabolomics of cancer. As a screening method, it can provide information about the state of health of patients. The main purpose of the study is to develop a highly reliable enantioanalysis method for the determination of D-, and L-leucine in biological samples in order to establish their role as biomarkers in the diagnosis of breast cancer. Two enantioselective stochastic sensors based on N-methyl-fullero-pyrrolidine in graphite and graphene nanopowder pastes were designed, characterized, and validated for the enantioanalysis of leucine in whole blood. Different signatures were recorded for the biomarkers when the stochastic sensors were used, proving their enantioselectivity. In addition, limits for detection on the order of ag L⁻¹ were recorded for each of the enantiomers of leucine when the proposed enantioselective stochastic sensors were used. The wide linear concentration ranges facilitated the assay of the L-leucine in healthy volunteers, and also in patients confirmed with breast cancer. Recoveries of one enantiomer in the presence of the other enantiomer in whole blood samples, higher than 96.50%, proved that the enantioanalysis of enantiomers can be performed reliably from whole blood samples. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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12 pages, 2453 KiB

Open AccessArticle

Electrochemical Detection of Surfactant-Encapsulated Aqueous Nanodroplets in Organic Solution

by Pankyu Kim, Hyeongkwon Moon and Jun Hui Park

Chemosensors 2023, 11(2), 112; https://doi.org/10.3390/chemosensors11020112 - 3 Feb 2023

Cited by 3 | Viewed by 1674

Abstract

We report enhanced electrochemical detection of single water-in-oil emulsion droplets using the nano-impact method. To detect the emulsion droplets, the water molecules in the droplets were directly oxidized (i.e., water splitting) without additional electroactive species when the droplets collided with the ultramicroelectrode. The [...] Read more.

We report enhanced electrochemical detection of single water-in-oil emulsion droplets using the nano-impact method. To detect the emulsion droplets, the water molecules in the droplets were directly oxidized (i.e., water splitting) without additional electroactive species when the droplets collided with the ultramicroelectrode. The water molecules in the emulsion droplet cannot be directly electrolyzed in an organic solvent because the emulsifier does not require a hydrophobic electrolyte. To enhance the signal intensity, the electrochemistry of sub-microscale single droplets was investigated considering the charge neutrality and limiting reagent. Therefore, effective electrolysis of the droplets was achieved. Approximately 10% of water molecules in the droplet (55.6 M H₂O) were oxidized based on calculations from the electrochemical peak analysis and DLS measurements. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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15 pages, 3300 KiB

Open AccessArticle

Smart Sensor for Lithium Detection: An Environmental Application

by Ilaria Antonia Vitale, Giulia Selvolini and Giovanna Marrazza

Chemosensors 2023, 11(2), 77; https://doi.org/10.3390/chemosensors11020077 - 19 Jan 2023

Cited by 1 | Viewed by 3398

Abstract

In this work, we propose a potentiometric smart sensor for lithium detection in environmental samples based on a screen-printed cell. The graphite screen-printed electrode (GSPE) was first modified by gold and silver nanoparticles to increase the conductivity, and then by an ion-selective membrane, [...] Read more.

In this work, we propose a potentiometric smart sensor for lithium detection in environmental samples based on a screen-printed cell. The graphite screen-printed electrode (GSPE) was first modified by gold and silver nanoparticles to increase the conductivity, and then by an ion-selective membrane, which was directly deposited onto the nanostructured electrode surface. The potentiometric cell, thanks to its small size, was integrated with a portable instrument connected to a smartphone for decentralized analysis. The developed sensor was used in drop- and microflow-configurations and showed a high sensitivity for lithium with a low detection limit (1.6 µM). It was also applied in the analysis of real samples from the industrial recycling of automotive batteries and complex matrices, such as contaminated soils. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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16 pages, 4243 KiB

Open AccessArticle

Bulk Modification of Sonogel–Carbon with Polyaniline: A Suitable Redox Mediator for Chlorophenols Detection

by Paloma Calatayud-Macías, David López-Iglesias, Alfonso Sierra-Padilla, Laura Cubillana-Aguilera, José María Palacios-Santander and Juan José García-Guzmán

Chemosensors 2023, 11(1), 63; https://doi.org/10.3390/chemosensors11010063 - 13 Jan 2023

Cited by 3 | Viewed by 1590

Abstract

In this work, the development and characterization of a new ceramic material modified with polyaniline powder obtained by a high-power ultrasound sol-gel route is presented. A preliminary screening of the conducting polymer electroactivity was performed by means of cyclic voltammetry in free analyte [...] Read more.

In this work, the development and characterization of a new ceramic material modified with polyaniline powder obtained by a high-power ultrasound sol-gel route is presented. A preliminary screening of the conducting polymer electroactivity was performed by means of cyclic voltammetry in free analyte solution. Remarkable figures of merit for 4-chloro-3-methylphenol (PCMC) determination, selected as the model organic analyte, was obtained with the developed material: the sensitivity and the limit of detection were 2.40 μA/μM·cm² and 0.69 μM, respectively. The developed device was also successfully applied in the electrochemical determination of PCMC in water samples collected from different sources, obtaining recovery values ranging from 92% to 105%. The electrochemical performance of the device for the detection of other chlorophenols of interest was better in comparison with the bare electrode in all cases, due to the presence of the bulk modifier in the material. Therefore, the electrode material can be promoted for electrochemical assays of different chlorophenols in buffer and real water media for environmental monitoring. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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11 pages, 2815 KiB

Open AccessArticle

Potentiometric Sensor System with Self-Calibration for Long-Term, In Situ Measurements

by Zhehao Zhang, Elena Boselli and Ian Papautsky

Chemosensors 2023, 11(1), 48; https://doi.org/10.3390/chemosensors11010048 - 5 Jan 2023

Viewed by 1883

Abstract

We built an integrated solid-contact ion-selective electrode (SCISE) system with the functionality of self-calibration. A multiplexed SCISE sensor (K⁺ and NO₃⁻ vs. Ag/AgCl) was fabricated on printed-circuit board (PCB) substrates and was subsequently embedded into a microfluidic flow cell for [...] Read more.

We built an integrated solid-contact ion-selective electrode (SCISE) system with the functionality of self-calibration. A multiplexed SCISE sensor (K⁺ and NO₃⁻ vs. Ag/AgCl) was fabricated on printed-circuit board (PCB) substrates and was subsequently embedded into a microfluidic flow cell for self-calibration and flow-through analysis. A PCB circuit that includes modules for both sensor readout and fluid control was developed. The sensors showed a fast and near-Nernstian response (56.6 for the K⁺ electrode and −57.4 mV/dec for the NO₃⁻ electrode) and maintained their performance for at least three weeks. The sensors also showed a highly reproducible response in an automated two-point calibration, demonstrating the potential for in situ monitoring. Lastly, the sensor system was successfully applied to measure mineral nutrients in plant sap samples. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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14 pages, 3494 KiB

Open AccessArticle

Potentiometric Surfactant Sensor for Anionic Surfactants Based on 1,3-dioctadecyl-1H-imidazol-3-ium tetraphenylborate

by Nikola Sakač, Dubravka Madunić-Čačić, Dean Marković, Lucija Hok, Robert Vianello, Valerije Vrček, Bojan Šarkanj, Bojan Đurin, Bartolomeo Della Ventura, Raffaele Velotta and Marija Jozanović

Chemosensors 2022, 10(12), 523; https://doi.org/10.3390/chemosensors10120523 - 8 Dec 2022

Cited by 3 | Viewed by 1400

Abstract

As anionic surfactants are used as cleaning agents, they pose an environmental and health threat. A novel potentiometric sensor for anionic surfactants based on the 1,3-dioctadecyl-1H-imidazol-3-ium tetraphenylborate (DODI–TPB) ionophore is presented. The newly developed approach for DODI–TPB synthesis is faster and [...] Read more.

As anionic surfactants are used as cleaning agents, they pose an environmental and health threat. A novel potentiometric sensor for anionic surfactants based on the 1,3-dioctadecyl-1H-imidazol-3-ium tetraphenylborate (DODI–TPB) ionophore is presented. The newly developed approach for DODI–TPB synthesis is faster and simpler than the currently used strategies and follows the green chemistry principles. The DODI–TPB ionophore was characterized by computational and instrumental techniques (NMR, LC–MS, FTIR, elemental analysis) and used to produce a PVC-based DODI–TPB sensor. The sensor showed linear response to dodecylbenzenesulfonate and dodecyl sulfate in concentration ranges of 6.3 × 10⁻⁷–3.2 × 10⁻⁴ M and 5.9 × 10⁻⁷–4.1 × 10⁻³ M, for DBS and SDS, respectively. The sensor exhibits a Nernstian slope (59.3 mV/decade and 58.3 mV/decade for DBS and SDS, respectively) and low detection limits (7.1 × 10⁻⁷ M and 6.8 × 10⁻⁷ M for DBS and SDS, respectively). The DODI–TPB sensor was successfully tested on real samples of commercial detergents and the results are in agreement with the referent methods. A computational analysis underlined the importance of long alkyl chains in DODI⁺ and their C–H∙∙∙π interactions with TPB⁻ for the ionophore formation in solution, thereby providing guidelines for the future design of efficient potentiometric sensors. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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15 pages, 7850 KiB

Open AccessArticle

Ultrathin PANI-Decorated, Highly Purified and Well Dispersed Array Cncs for Highly Sensitive HCHO Sensors

by Qingmin Hu, Zhiheng Ma, Jie Yang, Tiange Gao, Yue Wu, Zhe Dong, Xuyi Li, Wen Zeng, Shichao Zhao and Jiaqiang Xu

Chemosensors 2021, 9(10), 276; https://doi.org/10.3390/chemosensors9100276 - 28 Sep 2021

Cited by 3 | Viewed by 2061

Abstract

The flocculation of small surficial groups on pristine CNCs (carbon nanocoils) bundles limit their application. In this study, we designed and fabricated novel array CNCs with a surficial decoration of polyaniline (PANI) using in situ methods. Atomic layer deposition (ALD) and chemical vapor [...] Read more.

The flocculation of small surficial groups on pristine CNCs (carbon nanocoils) bundles limit their application. In this study, we designed and fabricated novel array CNCs with a surficial decoration of polyaniline (PANI) using in situ methods. Atomic layer deposition (ALD) and chemical vapor deposition (CVD) methods were employed to fabricate the highly pure array CNCs. The array CNCs decorated with ultra-thin PANI were confirmed by different characterizations. Furthermore, this material displayed a good performance in its detection of formaldehyde. The detection results showed that the CNCs coated with PANI had a low limit of detection of HCHO, as low as 500 ppb, and the sensor also showed good selectivity for other interfering gases, as well as good repeatability over many tests. Furthermore, after increasing the PANI loading on the surface of the CNCs, their detection performance exhibited a typical volcanic curve, and the value of the enthalpy was extracted by using the temperature-varying micro-gravimetric method during the process of detection of the formaldehyde molecules on the CNCs. The use of array CNCs with surficial decoration offers a novel method for the application of CNCs and could be extended to other applications, such as catalysts and energy conversion. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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Review

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32 pages, 2712 KiB

Open AccessReview

Electrochemical Sensors for Liquid Biopsy and Their Integration into Lab-on-Chip Platforms: Revolutionizing the Approach to Diseases

by Salma Umme, Giulia Siciliano, Elisabetta Primiceri, Antonio Turco, Iolena Tarantini, Francesco Ferrara and Maria Serena Chiriacò

Chemosensors 2023, 11(10), 517; https://doi.org/10.3390/chemosensors11100517 - 1 Oct 2023

Cited by 2 | Viewed by 2190

Abstract

The screening and early diagnosis of diseases are crucial for a patient’s treatment to be successful and to improve their survival rate, especially for cancer. The development of non-invasive analytical methods able to detect the biomarkers of pathologies is a critical point to [...] Read more.

The screening and early diagnosis of diseases are crucial for a patient’s treatment to be successful and to improve their survival rate, especially for cancer. The development of non-invasive analytical methods able to detect the biomarkers of pathologies is a critical point to define a successful treatment and a good outcome. This study extensively reviews the electrochemical methods used for the development of biosensors in a liquid biopsy, owing to their ability to provide a rapid response, precise detection, and low detection limits. We also discuss new developments in electrochemical biosensors, which can improve the specificity and sensitivity of standard analytical procedures. Electrochemical biosensors demonstrate remarkable sensitivity in detecting minute quantities of analytes, encompassing proteins, nucleic acids, and circulating tumor cells, even within challenging matrices such as urine, serum, blood, and various other body fluids. Among the various detection techniques used for the detection of cancer biomarkers, even in the picogram range, voltammetric sensors are deeply discussed in this review because of their advantages and technical characteristics. This widespread utilization stems from their ability to facilitate the quantitative detection of ions and molecules with exceptional precision. A comparison of each electrochemical technique is discussed to assist with the selection of appropriate analytical methods. Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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29 pages, 7976 KiB

Open AccessReview

Surface Plasmon Electrochemistry: Tutorial and Review

by Zohreh Hirbodvash and Pierre Berini

Chemosensors 2023, 11(3), 196; https://doi.org/10.3390/chemosensors11030196 - 19 Mar 2023

Cited by 2 | Viewed by 2216

Abstract

Surface plasmon polaritons (SPPs) are optical surface waves propagating along a metal surface. They exhibit attributes such as field enhancement and sub-wavelength localization, which make them attractive for surface sensing, as they are heavily exploited in surface plasmon biosensors. Electrochemistry also occurs on [...] Read more.

Surface plasmon polaritons (SPPs) are optical surface waves propagating along a metal surface. They exhibit attributes such as field enhancement and sub-wavelength localization, which make them attractive for surface sensing, as they are heavily exploited in surface plasmon biosensors. Electrochemistry also occurs on metal surfaces, and electrochemical techniques are also commonly applied in biosensors. As metal surfaces are integral in both, it is natural to combine these techniques into a single platform. Motivations include: (i) realising a multimodal biosensor (electrochemical and optical), (ii) using SPPs to probe the electrochemical double layer or to probe electrochemical activity, thus revealing complementary information on redox reactions, or (iii) using SPPs to pump electrochemical reactions by creating non-equilibrium energetic electrons and holes in a working electrode through the absorption of SPPs thereon. The latter is of interest as it may yield novel redox reaction pathways (i.e., plasmonic electrocatalysis). Full article

(This article belongs to the Special Issue Recent Developments in Electrochemical Sensing)

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