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Chemosensors, Volume 10, Issue 3 (March 2022) – 31 articles

Cover Story (view full-size image): A simple, fast, sensitive and low-cost voltammetric method using a screen-printed carbon electrode (SPCE) is presented for the simultaneous determination of ascorbic acid (AA), paracetamol (PA), dextromethorphan (DX) and caffeine (CF) in both pharmaceutical formulations and samples of environmental interest. Well-defined and separated voltammetric peaks were obtained for all analytes, achieving limits of detection at the level of a few mg L−1. The developed differential pulse voltammetric (DPV) method was validated using both a pharmaceutical product and a spiked well water sample. A very good agreement between the determined and the theoretical label drug content and recoveries in the range of 99.5–100.8% were obtained for pharmaceutical product and well water samples, respectively. View this paper
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Article
Optical Response of CVD-Grown ML-WS2 Flakes on an Ultra-Dense Au NP Plasmonic Array
Chemosensors 2022, 10(3), 120; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030120 - 21 Mar 2022
Viewed by 1046
Abstract
The combination of metallic nanostructures with two-dimensional transition metal dichalcogenides is an efficient way to make the optical properties of the latter more appealing for opto-electronic applications. In this work, we investigate the optical properties of monolayer WS2 flakes grown by chemical [...] Read more.
The combination of metallic nanostructures with two-dimensional transition metal dichalcogenides is an efficient way to make the optical properties of the latter more appealing for opto-electronic applications. In this work, we investigate the optical properties of monolayer WS2 flakes grown by chemical vapour deposition and transferred onto a densely-packed array of plasmonic Au nanoparticles (NPs). The optical response was measured as a function of the thickness of a dielectric spacer intercalated between the two materials and of the system temperature, in the 75–350 K range. We show that a weak interaction is established between WS2 and Au NPs, leading to temperature- and spacer-thickness-dependent coupling between the localized surface plasmon resonance of Au NPs and the WS2 exciton. We suggest that the closely-packed morphology of the plasmonic array promotes a high confinement of the electromagnetic field in regions inaccessible by the WS2 deposited on top. This allows the achievement of direct contact between WS2 and Au while preserving a strong connotation of the properties of the two materials also in the hybrid system. Full article
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Article
The Effect of Thin Film Fabrication Techniques on the Performance of rGO Based NO2 Gas Sensors at Room Temperature
Chemosensors 2022, 10(3), 119; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030119 - 21 Mar 2022
Viewed by 1070
Abstract
Reduced graphene oxide (rGO) has attracted enormous interest as a promising candidate material for gas detection due to its large specific surface areas. In our work, rGO films were fabricated on a large scale using dip-coating and spin-coating methods for the detection of [...] Read more.
Reduced graphene oxide (rGO) has attracted enormous interest as a promising candidate material for gas detection due to its large specific surface areas. In our work, rGO films were fabricated on a large scale using dip-coating and spin-coating methods for the detection of nitrogen dioxide (NO2) gas at room temperature. The influence of different test environments on the sensing performance, including the test atmosphere, gas flow and gas pressure was evaluated. The response time of the dip-coating method was 573 s with a long recovery period of 639 s and for the spin-coating method, the response time and recovery time was 386 s and 577 s, respectively. In addition, the spin-coated sensor exhibited high selectivity to NO2, with the response increasing by more than 20% (for 15 ppm NO2) as compared with that for HCHO, NH3, and CH4. Our results indicated that the spin coating method was more suitable for rGO-based gas sensors with higher performance. Full article
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Article
Assessing over Time Performance of an eNose Composed of 16 Single-Type MOX Gas Sensors Applied to Classify Two Volatiles
Chemosensors 2022, 10(3), 118; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030118 - 19 Mar 2022
Viewed by 758
Abstract
This paper assesses the over time performance of a custom electronic nose (eNose) composed of an array of commercial low-cost and single-type miniature metal-oxide (MOX) semiconductor gas sensors. The eNose uses 16 BME680 versatile sensor devices, each including an embedded non-selective MOX gas [...] Read more.
This paper assesses the over time performance of a custom electronic nose (eNose) composed of an array of commercial low-cost and single-type miniature metal-oxide (MOX) semiconductor gas sensors. The eNose uses 16 BME680 versatile sensor devices, each including an embedded non-selective MOX gas sensor that was originally proposed to measure the total volatile organic compounds (TVOC) in the air. This custom eNose has been used previously to detect ethanol and acetone, obtaining initial promising classification results that worsened over time because of sensor drift. The current paper assesses the over time performance of different classification methods applied to process the information gathered from the eNose. The best classification results have been obtained when applying a linear discriminant analysis (LDA) to the normalized conductance of the sensing layer of the 16 MOX gas sensors available in the eNose. The LDA procedure by itself has reduced the influence of drift in the classification performance of this single-type eNose during an evaluation period of three months. Full article
(This article belongs to the Special Issue Advances in Analytical Systems for Gaseous Mixture)
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Review
A Review on the Use of Biochar Derived Carbon Quantum Dots Production for Sensing Applications
Chemosensors 2022, 10(3), 117; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030117 - 19 Mar 2022
Cited by 1 | Viewed by 964
Abstract
Since their discovery, carbon dots have attracted a great deal of interest for their perspective biological applications. Nevertheless, the quenching of carbon dots photoluminescence represents an interesting feature for quantitative analysis in very low concentration of many species. A particular approach for the [...] Read more.
Since their discovery, carbon dots have attracted a great deal of interest for their perspective biological applications. Nevertheless, the quenching of carbon dots photoluminescence represents an interesting feature for quantitative analysis in very low concentration of many species. A particular approach for the production of carbon dots is the use of biochar, a carbonized biomass, as a precursor. In this work, we overview the main achievements accomplished by using biochar-derived carbon dots for detecting and quantifying inorganic and organic species. We also provide background knowledge of the main properties, production and purification routes of carbon dots. Full article
(This article belongs to the Special Issue Biochar Based Sustainable Sensing Platforms)
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Article
Dynamic Potentiometry with an Ion-Selective Electrode: A Tool for Qualitative and Quantitative Analysis of Inorganic and Organic Cations
Chemosensors 2022, 10(3), 116; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030116 - 18 Mar 2022
Viewed by 824
Abstract
A study of the transient potential signals obtained with a cation-selective electrode based on an ion-exchanger was carried out for solutions of the following individual cations at different concentrations: H+, Li+, Na+, K+, Rb+ [...] Read more.
A study of the transient potential signals obtained with a cation-selective electrode based on an ion-exchanger was carried out for solutions of the following individual cations at different concentrations: H+, Li+, Na+, K+, Rb+, Mg2+, Ca2+, choline (Ch+), acetylcholine (AcCh+), and procaine (Pr+). Three different general types of transient signals were distinguished depending on the value of the selectivity coefficient of the corresponding ion. A principal component analysis (PCA) was performed on the signals, finding that the qualitative identification of the corresponding ion from the scores of two principal components is possible. The study was extended to the transient signals of solutions containing an analyte in the presence of an interfering ion. The PCA of the corresponding signal allows for the detection of the presence of interfering ions, thus avoiding biased results in the determination of the analyte. Moreover, the two principal components of the transient signals obtained for each of the ions at different concentrations allow for the construction of calibration graphs for the quantitative determination of the corresponding ion. All the transient signals obtained experimentally in this work can be reconstructed accurately from principal components and their corresponding scores. Full article
(This article belongs to the Special Issue Modern Directions in Ion Electroanalysis for Real World Applications)
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Article
Perchlorate Solid-Contact Ion-Selective Electrode Based on Dodecabenzylbambus[6]uril
Chemosensors 2022, 10(3), 115; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030115 - 18 Mar 2022
Cited by 1 | Viewed by 821
Abstract
Dodecabenzylbambus[6]uril (Bn12BU[6]) is an anion receptor that binds the perchlorate ion the most tightly (stability constant ~1010 M−1) of all anions due to the excellent match between the ion size in relation to the receptor cavity. This new bambusuril compound was used as [...] Read more.
Dodecabenzylbambus[6]uril (Bn12BU[6]) is an anion receptor that binds the perchlorate ion the most tightly (stability constant ~1010 M−1) of all anions due to the excellent match between the ion size in relation to the receptor cavity. This new bambusuril compound was used as an ionophore in the ion-selective membrane (ISM) to develop ion selective electrodes (ISEs) for determination of perchlorate concentration utilizing the poly(3,4-ethylenedioxythiophene) (PEDOT) polymer film as a solid-contact material. Variation of the content of Bn12BU[6] and tridodecylmethylammonium chloride (TDMACl) in the plasticized poly(vinyl chloride)-based ISM was also tested. All the prepared solid-contact ISEs and their analytical performance were characterized by potentiometry, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and chronopotentiometry. The ISEs showed rapid response and a sub-Nernstian slope (~57 mV/decade) during potentiometric measurements in perchlorate solutions in the concentration range from 10−1 to 10−6 M simultaneously with their high stability and sufficient selectivity to other common inorganic anions like bromide, chloride, nitrate and sulphate. The function of the ISE was further verified by analysis of real water samples (lake, sea, and mineral water), which gave accurate and precise results. Full article
(This article belongs to the Special Issue Functionalized Materials for Chemosensor Applications)
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Article
Effect of Applied Electrical Stimuli to Interdigitated Electrode Sensors While Detecting 17α-Ethinylestradiol in Water Samples
Chemosensors 2022, 10(3), 114; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030114 - 16 Mar 2022
Cited by 1 | Viewed by 625
Abstract
The effect of impedance measurements of applied voltage on the detection of 17α-ethinylestradiol (EE2) in water samples using interdigitated electrodes (IDE) coated or not with thin films, is described. Firstly, the effect of immersion in EE2 aqueous solutions of layer-by-layer films prepared with [...] Read more.
The effect of impedance measurements of applied voltage on the detection of 17α-ethinylestradiol (EE2) in water samples using interdigitated electrodes (IDE) coated or not with thin films, is described. Firstly, the effect of immersion in EE2 aqueous solutions of layer-by-layer films prepared with poly(allylamine hydrochloride) (PAH), graphene oxide (GO), poly(1-(4-(3-carboxy-4-hydroxyphenylazo) benzene sulfonamido) 1,2 ethanediyl, sodium salt) (PAZO), polyethylenimine (PEI) and poly(sodium 4-styrenesulfonate) (PSS) was analyzed. These results demonstrated that PAH/GO films desorb during the immersion on EE2 solutions, while EE2 adsorbs on PAH/PAZO and PEI/PSS films with characteristic time values of 16.7 and 7.1 min, respectively, demonstrating that both films are adequate for the development of EE2 sensors. However, as the adsorption characteristic time is shorter, and the EE2 adsorbed amount is smaller, the PEI/PSS films are more suitable for the development of sensors. The effect of the applied voltage was analyzed using both IDEs covered with PEI/PSS films as well as those uncoated. The capacitance spectra are best fitted to analyze this effect, and the loss tangent spectra are advantageous to analyze the aqueous media. Furthermore, it was concluded that lower voltage values are best suited to perform measurements of this nature, given that higher voltages lead to less reliable results and cause irreparable damage to the sensors. Full article
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Article
Carbon Dots from Coffee Grounds: Synthesis, Characterization, and Detection of Noxious Nitroanilines
Chemosensors 2022, 10(3), 113; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030113 - 15 Mar 2022
Viewed by 782
Abstract
Coffee ground (CG) waste is generated in huge amounts all over the world, constituting a serious environmental issue owing to its low biodegradability. Therefore, processes that simultaneously aim for its valorization while reducing its environmental impact are in great demand. In the current [...] Read more.
Coffee ground (CG) waste is generated in huge amounts all over the world, constituting a serious environmental issue owing to its low biodegradability. Therefore, processes that simultaneously aim for its valorization while reducing its environmental impact are in great demand. In the current approach, blue luminescent carbon dots (C-dots) were produced in good chemical yields from CGs following hydrothermal carbonization methods under an extended set of reaction parameters. The remarkable fluorescent properties of the synthesized C-dots (quantum yields up to 0.18) allied to their excellent water dispersibility and photostability prompted their use for the first time as sensing elements for detection of noxious nitroanilines (NAs) in aqueous media. Very high levels of NA detection were achieved (e.g., limit of detection of 68 ppb for p-nitroaniline), being the regioisomeric selectivity attributed to its higher hyperpolarizability and dipole moment. Through ground–state and time-resolved fluorescence assays, a static fluorescence quenching mechanism was established. 1H NMR titration data also strongly suggested the formation of ground–state complexes between C-dots and NAs. Full article
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Review
Recent Sensing Technologies of Imperceptible Water in Atmosphere
Chemosensors 2022, 10(3), 112; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030112 - 14 Mar 2022
Viewed by 768
Abstract
Accurate detection and quantitative evaluation of environmental water in vapor and liquids state expressed as humidity and precipitation play key roles in industrial and scientific applications. However, the development of supporting tools and techniques remains a challenge. Although optical methods such as IR [...] Read more.
Accurate detection and quantitative evaluation of environmental water in vapor and liquids state expressed as humidity and precipitation play key roles in industrial and scientific applications. However, the development of supporting tools and techniques remains a challenge. Although optical methods such as IR and LASER could detect environmental water in the air, their apparatus is relatively huge. Alternatively, solid detection field systems (SDFSs) could recently lead to a revolution in device downsizing and sensing abilities via advanced research, mainly for materials technology. Herein, we present an overview of several SDFS based sensing categories and their core materials mainly used to detect water in atmosphere, either in the vapor or liquid phase. We considered the governing mechanism in the detection process, such as adsorption/desorption, condensation/evaporation for the vapor phase, and surface attach/detach for the liquid phase. Sensing categories such as optical, chilled mirror, resistive, capacitive, gravimetric sensors were reviewed together with their designated tools such as acoustic wave, quartz crystal microbalance, IDT, and many others, giving typical examples of daily based real scientific applications. Full article
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Article
A Comparative Study of Aqueous and Non-Aqueous Solvents to Be Used in Low-Temperature Serial Molecular–Electronic Sensors
Chemosensors 2022, 10(3), 111; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030111 - 12 Mar 2022
Viewed by 767
Abstract
This paper presents the experimental results of studying the samples of the electrochemical sensors of motion parameters on the base of Molecular Electronics Technology (MET). The sensors with microelectromechanical (MEMS) electrode assembly use electrolytes based on aqueous and non-aqueous solutions of potassium and [...] Read more.
This paper presents the experimental results of studying the samples of the electrochemical sensors of motion parameters on the base of Molecular Electronics Technology (MET). The sensors with microelectromechanical (MEMS) electrode assembly use electrolytes based on aqueous and non-aqueous solutions of potassium and lithium iodides. Electrolyte solutions contain impurities of ionic liquids and alcohols to achieve stable low-temperature operation and acceptable technical parameters of serial devices. The dependence of the general sensitivity and the shape of the amplitude-frequency characteristic on temperature have been studied. For the marginally acceptable samples, which had an acceptable temperature dependence of the conversion coefficient and low activation energies for the diffusion coefficient, the level of self-noise was found. The activation energy of the electrolyte diffusion coefficient was determined based on the analysis of the dependence of the background current on temperature. A conclusion was made regarding the possible prospects for using the studied solutions and components for operation in serial devices. Full article
(This article belongs to the Special Issue Optical Chemical Sensors and Spectroscopy)
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Article
Femtosecond Direct Laser Writing of Silver Clusters in Phosphate Glasses for X-ray Spatially-Resolved Dosimetry
Chemosensors 2022, 10(3), 110; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030110 - 11 Mar 2022
Cited by 1 | Viewed by 803
Abstract
Radio-photoluminescence in silver-doped phosphate glasses has been extensively used for X-ray dosimetry. In this paper, we present the potential of silver clusters for X-ray spatially resolved dosimetry. Those clusters are generated in phosphate glasses containing a high concentration of silver oxide by femtosecond [...] Read more.
Radio-photoluminescence in silver-doped phosphate glasses has been extensively used for X-ray dosimetry. In this paper, we present the potential of silver clusters for X-ray spatially resolved dosimetry. Those clusters are generated in phosphate glasses containing a high concentration of silver oxide by femtosecond direct laser writing technique. Two phosphate glasses of different compositions were investigated. First, the spectroscopic properties of the pristine glasses were studied after X-ray irradiation at different doses to assess their dosimetry potential. Second, the impact of X-rays on the three-dimensional inscribed silver clusters has been analyzed using several spectroscopies methods. Our analysis highlights the resilience of embedded silver clusters acting as local probes of the deposited doses. We demonstrate that these inscribed glasses can define the range and sensitivity of X-ray doses and consider the realization of spatially-resolved dosimeters. Full article
(This article belongs to the Special Issue Optical Chemical Sensors and Spectroscopy)
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Communication
The SnO2/MXene Composite Ethanol Sensor Based on MEMS Platform
Chemosensors 2022, 10(3), 109; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030109 - 11 Mar 2022
Cited by 1 | Viewed by 973
Abstract
In recent years, two-dimensional layered material MXene has attracted extensive attention in the fields of sensors due to its large specific surface area and rich active sites. So, we employed multilayer Ti3C2TX and SnO2 microspheres to prepare [...] Read more.
In recent years, two-dimensional layered material MXene has attracted extensive attention in the fields of sensors due to its large specific surface area and rich active sites. So, we employed multilayer Ti3C2TX and SnO2 microspheres to prepare SnO2/MXene composites for enhancing gas-sensing properties of pristine SnO2. The composite was brushed on a microelectromechanical system (MEMS) platform to make resistance-type gas sensors with low power consumption. The gas-sensing results show that the SnO2/MXene sensor with the best composite ratio (SnO2: MXene mass ratio is 5:1, named SM-5) greatly improves gas sensitivity of SnO2 sensor, among which the sensitivity to ethanol gas is the highest. At the same time, the composite also speeds up the response recovery speed of the sensor. When the SM-5 sensor worked at its optimal temperature 230 °C, its response value to 10 ppm ethanol reaches 5.0, which is twice that of the pristine SnO2 sensor. Its response and recovery time are only 14 s and 26 s, respectively. The sensing mechanism of the composite is discussed according to the classical the space charge or depletion layer model. It is concluded that the Schottky barrier of composites and the metal properties of Ti3C2Tx are responsible for improvement of the gas-sensing properties of the composite. Full article
(This article belongs to the Special Issue 2D Materials for Gas Sensing)
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Article
Rapid On-Site Detection of Illicit Drugs in Smuggled Samples with a Portable Electrochemical Device
Chemosensors 2022, 10(3), 108; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030108 - 11 Mar 2022
Cited by 1 | Viewed by 955
Abstract
The smuggling of illicit drugs urges the development of new tools for rapid on-site identification in cargos. Current methods rely on presumptive color tests and portable spectroscopic techniques. However, these methods sometimes exhibit inaccurate results due to commonly used cutting agents, the colorful [...] Read more.
The smuggling of illicit drugs urges the development of new tools for rapid on-site identification in cargos. Current methods rely on presumptive color tests and portable spectroscopic techniques. However, these methods sometimes exhibit inaccurate results due to commonly used cutting agents, the colorful nature of the sample or because the drugs are smuggled in common goods. Interestingly, electrochemical sensors can deal with these specific problems. Herein, an electrochemical device is presented that uses affordable screen-printed electrodes for the electrochemical profiling of several illicit drugs by square-wave voltammetry (SWV). The identification of the illicit compound is based on the oxidation potential of the analyte. Hence, a library of electrochemical profiles is built upon the analysis of illicit drugs and common cutting agents. This library allows the design of a tailor-made script that enables the identification of each drug through a user-friendly interface (laptop or mobile phone). Importantly, the electrochemical test is compared by analyzing 48 confiscated samples with other portable devices based on Raman and FTIR spectroscopy as well as a laboratory standard method (i.e., gas chromatography–mass spectrometry). Overall, the electrochemical results, obtained through the analysis of different samples from confiscated cargos at an end-user site, present a promising alternative to current methods, offering low-cost and rapid testing in the field. Full article
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Article
Phosphorous (V) Corrole Fluorophores for Nitrite Assessment in Environmental and Biological Samples
Chemosensors 2022, 10(3), 107; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030107 - 10 Mar 2022
Viewed by 680
Abstract
Two phosphorous (V) corrole complexes, [5,10,15-pentafluorophenyl corrole] phosphorous (V) (PFCorr) and [10-(4-trimethylsilylphenyl)-5,15-dimesityl-corrole] phosphorous (V) (PCorr) were synthesized and tested as nitrite-sensitive fluorophores. Fluorimetry studies on ligand sensitivity towards anions were carried out in solution, then inside polymeric membrane optodes [...] Read more.
Two phosphorous (V) corrole complexes, [5,10,15-pentafluorophenyl corrole] phosphorous (V) (PFCorr) and [10-(4-trimethylsilylphenyl)-5,15-dimesityl-corrole] phosphorous (V) (PCorr) were synthesized and tested as nitrite-sensitive fluorophores. Fluorimetry studies on ligand sensitivity towards anions were carried out in solution, then inside polymeric membrane optodes deposited on glass, and finally by functionalized SiO2 nanoparticles deposited on a paper support. The selective fluorescence quenching was registered upon addition of an increasing amount of NO2 ions for both ligands. The influence on the PFCorr optode’s response of the lipophilic sites’ functionalization was investigated. The sensors’ suitability for nitrite assessment in natural waters at levels 10-fault lower than the WHO’s recommended maximum concentration level of 3 mg/L was demonstrated. Full article
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Review
Recent Advances in Quartz Crystal Microbalance Biosensors Based on the Molecular Imprinting Technique for Disease-Related Biomarkers
Chemosensors 2022, 10(3), 106; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030106 - 10 Mar 2022
Viewed by 780
Abstract
The molecular imprinting technique is a quickly developing field of interest regarding the synthesis of artificial recognition elements that enable the specific determination of target molecule/analyte from a matrix. Recently, these smart materials can be successfully applied to biomolecule detection in biomimetic biosensors. [...] Read more.
The molecular imprinting technique is a quickly developing field of interest regarding the synthesis of artificial recognition elements that enable the specific determination of target molecule/analyte from a matrix. Recently, these smart materials can be successfully applied to biomolecule detection in biomimetic biosensors. These biosensors contain a biorecognition element (a bioreceptor) and a transducer, like their biosensor analogs. Here, the basic difference is that molecular imprinting-based biosensors use a synthetic recognition element. Molecular imprinting polymers used as the artificial recognition elements in biosensor platforms are complementary in shape, size, specific binding sites, and functionality to their template analytes. Recent progress in biomolecular recognition has supplied extra diagnostic and treatment methods for various diseases. Cost-effective, more robust, and high-throughput assays are needed for monitoring biomarkers in clinical settings. Quartz crystal microbalance (QCM) biosensors are promising tools for the real-time and quick detection of biomolecules in the past two decades A quick, simple-to-use, and cheap biomarkers detection technology based on biosensors has been developed. This critical review presents current applications in molecular imprinting-based quartz crystal microbalance biosensors for the quantification of biomarkers for disease monitoring and diagnostic results. Full article
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Article
Fast GC E-Nose and Chemometrics for the Rapid Assessment of Basil Aroma
Chemosensors 2022, 10(3), 105; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030105 - 10 Mar 2022
Cited by 1 | Viewed by 667
Abstract
The aim of this work is to assess the potentialities of the synergistic combination of an ultra-fast chromatography-based electronic nose as a fingerprinting technique and multivariate data analysis in the context of food quality control and to investigate the influence of some factors, [...] Read more.
The aim of this work is to assess the potentialities of the synergistic combination of an ultra-fast chromatography-based electronic nose as a fingerprinting technique and multivariate data analysis in the context of food quality control and to investigate the influence of some factors, i.e., basil variety, cut, and year of crop, in the final aroma of the samples. A low = level data fusion approach coupled with Principal Component Analysis (PCA) and ANOVA—Simultaneous Component Analysis (ASCA) was used in order to analyze the chromatographic signals acquired with two different columns (MXT-5 and MXT-1701). While the PCA analysis results highlighted the peculiarity of some basil varieties, differing either by a higher concentration of some of the detected chemical compounds or by the presence of different compounds, the ASCA analysis pointed out that variety and year are the most relevant effects, and also confirmed the results of previous investigations. Full article
(This article belongs to the Special Issue Chemometrics for Multisensor Systems and Artificial Senses)
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Communication
Dielectrophoresis-Based Biosensor for Detection of the Cancer Biomarkers CEA and CA 242 in Serum
Chemosensors 2022, 10(3), 104; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030104 - 10 Mar 2022
Viewed by 635
Abstract
We show that dielectrophoresis (DEP) spectroscopy is an effective transduction mechanism for detection of the concentration levels of the pancreatic cancer biomarkers cancer antigen (CA) 242 and carcinoembryonic antigen (CEA) in serum. We noticed a frequency dependence of the negative DEP force applied [...] Read more.
We show that dielectrophoresis (DEP) spectroscopy is an effective transduction mechanism for detection of the concentration levels of the pancreatic cancer biomarkers cancer antigen (CA) 242 and carcinoembryonic antigen (CEA) in serum. We noticed a frequency dependence of the negative DEP force applied by interdigitated electrodes on functionalized polystyrene microspheres (PM) with respect to changes in the number of these cancer antigens bound to the PM. An electrode array with a well-defined gradient of the electric field was designed and used, which enabled the automation of the signal processing and reproducibility of the signal acquired by the biosensor. Full article
(This article belongs to the Special Issue Feature Papers on Optical Chemical Sensors and Biosensors)
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Review
Inkjet Printing: A Viable Technology for Biosensor Fabrication
Chemosensors 2022, 10(3), 103; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030103 - 09 Mar 2022
Cited by 2 | Viewed by 952
Abstract
Printing technology promises a viable solution for the low-cost, rapid, flexible, and mass fabrication of biosensors. Among the vast number of printing techniques, screen printing and inkjet printing have been widely adopted for the fabrication of biosensors. Screen printing provides ease of operation [...] Read more.
Printing technology promises a viable solution for the low-cost, rapid, flexible, and mass fabrication of biosensors. Among the vast number of printing techniques, screen printing and inkjet printing have been widely adopted for the fabrication of biosensors. Screen printing provides ease of operation and rapid processing; however, it is bound by the effects of viscous inks, high material waste, and the requirement for masks, to name a few. Inkjet printing, on the other hand, is well suited for mass fabrication that takes advantage of computer-aided design software for pattern modifications. Furthermore, being drop-on-demand, it prevents precious material waste and offers high-resolution patterning. To exploit the features of inkjet printing technology, scientists have been keen to use it for the development of biosensors since 1988. A vast number of fully and partially inkjet-printed biosensors have been developed ever since. This study presents a short introduction on the printing technology used for biosensor fabrication in general, and a brief review of the recent reports related to virus, enzymatic, and non-enzymatic biosensor fabrication, via inkjet printing technology in particular. Full article
(This article belongs to the Special Issue Feature Papers on Optical Chemical Sensors and Biosensors)
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Article
A Portable Battery-Operated Sensor System for Simple and Rapid Assessment of Virgin Olive Oil Quality Grade
Chemosensors 2022, 10(3), 102; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030102 - 09 Mar 2022
Viewed by 631
Abstract
Virgin olive oil quality is assessed by chemical as well as sensory analysis. Two of the most important parameters that define the quality of virgin olive oils are the free acidity and the peroxide index. These chemical parameters are usually determined by manual [...] Read more.
Virgin olive oil quality is assessed by chemical as well as sensory analysis. Two of the most important parameters that define the quality of virgin olive oils are the free acidity and the peroxide index. These chemical parameters are usually determined by manual titration procedures that must be carried out in a laboratory by trained personnel. In this paper, a portable sensor system to support the quality grade assessment of virgin olive oil is presented. The system is battery operated and characterized by small dimensions, light weight and quick measurement response (about 30 s). The working principle is based on the measurement of the electrical conductance of an emulsion between a chemical reagent and the olive oil sample. Two different chemical reagents have been investigated: (1) a hydro-alcoholic solution (HAS), made of 60% ethanol and 40% distilled water; (2) 100% distilled water (DW). Tests have been carried out on a set of 40 olive oil samples. The results have shown how, for most of the fresh virgin olive oil samples (31 samples out of 40), the free acidity can be estimated with good accuracy from the electrical conductance of the emulsion using HAS as the reagent. In the case of the full set of samples, the emulsion electrical conductance, using HAS as the reagent, is a function of both the sample free acidity as well as the compounds produced by oil oxidation, and a compensation method based on the measured electrical conductance, using DW as the reagent, has been introduced to improve the accuracy in the estimated free acidity. Tests have also been carried out on the full set of samples, using a k-nearest neighbors algorithm, to demonstrate the feasibility of olive oil classification according to the quality grade. The results have shown how measurements carried out using only the HAS reagent provide better classification accuracy than measurements carried out using both the HAS and DW reagents. The proposed system can be a low-cost alternative to standard laboratory analyses to evaluate the quality grade of virgin olive oil. Full article
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Article
Surface-Enhanced Raman Spectroscopy for the Investigation of Chromogenic Motion Picture Films: A Preliminary Study
Chemosensors 2022, 10(3), 101; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030101 - 06 Mar 2022
Viewed by 802
Abstract
In the present work, surface-enhanced Raman spectroscopy (SERS) is proposed for the identification of dyes in chromogenic films. These substances, which are generated within the film itself during the colour development process, are first studied on reference molecules synthesised for the purpose and, [...] Read more.
In the present work, surface-enhanced Raman spectroscopy (SERS) is proposed for the identification of dyes in chromogenic films. These substances, which are generated within the film itself during the colour development process, are first studied on reference molecules synthesised for the purpose and, subsequently, on dyes extracted from a chromogenic film. SERS spectroscopy proved to be an efficient technique for their investigation, providing a proof of concept for its applicability for further studies on this complex topic. SERS spectra of the reference molecules were also compared with normal Raman spectra, acquired with a spectrometer based on SSE™ technology. Furthermore, the excellent SERS properties of anisotropic nanomaterials, such as silver nanostars, have been confirmed. Full article
(This article belongs to the Special Issue SERS: Analytical and Biological Challenges)
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Article
A Label-Free Colorimetric Assay Based on Gold Nanoparticles for the Detection of H2O2 and Glucose
Chemosensors 2022, 10(3), 100; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030100 - 05 Mar 2022
Viewed by 752
Abstract
The significance of sensing hydrogen peroxide (H2O2) is due to its ubiquity, being a potential biomarker as well as an end-product of several oxidation reactions. Herein, based on gold nanoparticles (AuNPs) and coupled with single-stranded DNA (ssDNA) and ceria [...] Read more.
The significance of sensing hydrogen peroxide (H2O2) is due to its ubiquity, being a potential biomarker as well as an end-product of several oxidation reactions. Herein, based on gold nanoparticles (AuNPs) and coupled with single-stranded DNA (ssDNA) and ceria nanoparticles (CeO2), we developed a novel colorimetric method to detect H2O2 and glucose in NaCl solutions. In the presence of H2O2, ssDNA adsorbed on the surface of CeO2 could be released and subsequently decorated AuNPs, resulting in a distinct color change of the aqueous solution from purple to red, which could be observed by the naked eye. Since H2O2 can be produced in the process of glucose oxidation by glucose oxidase (GOx), this approach can also be employed to detect glucose. By employing this sensing system, the detection limits for H2O2 and glucose are about 0.21 μM and 3.01 µM, respectively. Additionally, monitoring the content of glucose in blood serum samples was successfully achieved by the proposed strategy. This work opens a potential avenue for the quantitative detection of H2O2 and glucose in clinical diagnostics. Full article
(This article belongs to the Special Issue Feature Papers on Luminescent Sensing)
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Article
Red-Emitting Polymerizable Guanidinium Dyes as Fluorescent Probes in Molecularly Imprinted Polymers for Glyphosate Detection
Chemosensors 2022, 10(3), 99; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030099 - 03 Mar 2022
Viewed by 953
Abstract
The development of methodologies to sense glyphosate has gained momentum due to its toxicological and ecotoxicological effects. In this work, a red-emitting and polymerizable guanidinium benzoxadiazole probe was developed for the fluorescence detection of glyphosate. The interaction of the fluorescent probe and the [...] Read more.
The development of methodologies to sense glyphosate has gained momentum due to its toxicological and ecotoxicological effects. In this work, a red-emitting and polymerizable guanidinium benzoxadiazole probe was developed for the fluorescence detection of glyphosate. The interaction of the fluorescent probe and the tetrabutylammonium salt of glyphosate was studied via UV/vis absorption and fluorescence spectroscopy in chloroform and acetonitrile. The selective recognition of glyphosate was achieved by preparing molecularly imprinted polymers, able to discriminate against other common herbicides such as 2,4-dichlorophenoxyacetic acid (2,4-D) and 3,6-dichloro-2-methoxybenzoic acid (dicamba), as thin layers on submicron silica particles. The limits of detection of 4.8 µM and 0.6 µM were obtained for the sensing of glyphosate in chloroform and acetonitrile, respectively. The reported system shows promise for future application in the sensing of glyphosate through further optimization of the dye and the implementation of a biphasic assay with water/organic solvent mixtures for sensing in aqueous environmental samples. Full article
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Article
Cucurbit[8]uril-Based Potentiometric Sensor Coupled to HPLC for Determination of Tetracycline Residues in Milk Samples
Chemosensors 2022, 10(3), 98; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030098 - 03 Mar 2022
Viewed by 820
Abstract
The determination of chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples by HPLC coupled to a cucurbit[8]uril-based potentiometric sensor is herein presented. The new tetracycline-selective electrode is based on a polymeric membrane incorporating cucurbit[8]uril as a macrocyclic host, potassium tetrakis(p-chlorophenyl) borate as an [...] Read more.
The determination of chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples by HPLC coupled to a cucurbit[8]uril-based potentiometric sensor is herein presented. The new tetracycline-selective electrode is based on a polymeric membrane incorporating cucurbit[8]uril as a macrocyclic host, potassium tetrakis(p-chlorophenyl) borate as an ionic additive, 2-fluorophenyl 2-nitrophenyl ether as a plasticizer, and multi-walled carbon nanotubes as nanostructured materials. A microfluidic wall-jet flow-cell is implemented as a potentiometric detector after chromatographic separation by a C8 column using a gradient mobile phase of sulphuric acid and acetonitrile. The proposed methodology was validated following International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) and European Union (EU) guidelines. Linear regression models provided R2 in the range from 0.9973 ± 0.0026 to 0.9987 ± 0.0012 for all tetracycline antibiotics. The limits of detection and quantification ranged from 13.3 to 46.0 μg L−1 and 44.4 to 92.1 μg L−1, respectively. Precision intra-day, inter-day, and inter-electrode showed relative standard deviation values lower than 12.5%, 13.5%, and 12.9%, respectively. Accuracy was assessed by analysis of spiked milk samples around the maximum residue limit, yielding recovery values in the range from 81.3 to 108.5%. The simple, sensitive, cost-effective, and reliable HPLC-ion-selective electrode method justifies its use as a competitive alternative for the analysis of tetracycline residues in the food quality control sector. Full article
(This article belongs to the Special Issue Modern Directions in Ion Electroanalysis for Real World Applications)
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Review
Flexible Sensors Based on Conductive Polymers
Chemosensors 2022, 10(3), 97; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030097 - 01 Mar 2022
Cited by 1 | Viewed by 1402
Abstract
Conductive polymers have attracted wide attention since their discovery due to their unique properties such as good electrical conductivity, thermal and chemical stability, and low cost. With different possibilities of preparation and deposition on surfaces, they present unique and tunable structures. Because of [...] Read more.
Conductive polymers have attracted wide attention since their discovery due to their unique properties such as good electrical conductivity, thermal and chemical stability, and low cost. With different possibilities of preparation and deposition on surfaces, they present unique and tunable structures. Because of the ease of incorporating different elements to form composite materials, conductive polymers have been widely used in a plethora of applications. Their inherent mechanical tolerance limit makes them ideal for flexible devices, such as electrodes for batteries, artificial muscles, organic electronics, and sensors. As the demand for the next generation of (wearable) personal and flexible sensing devices is increasing, this review aims to discuss and summarize the recent manufacturing advances made on flexible electrochemical sensors. Full article
(This article belongs to the Special Issue Smart Polymer-Based Chemical and Biological Sensors)
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Article
Porous Pb-Doped ZnO Nanobelts with Enriched Oxygen Vacancies: Preparation and Their Chemiresistive Sensing Performance
Chemosensors 2022, 10(3), 96; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030096 - 01 Mar 2022
Cited by 1 | Viewed by 748
Abstract
Among various approaches to improve the sensing performance of metal oxide, the metal-doped method is perceived as effective, and has received great attention and is widely investigated. However, it is still a challenge to construct heterogeneous metal-doped metal oxide with an excellent sensing [...] Read more.
Among various approaches to improve the sensing performance of metal oxide, the metal-doped method is perceived as effective, and has received great attention and is widely investigated. However, it is still a challenge to construct heterogeneous metal-doped metal oxide with an excellent sensing performance. In the present study, porous Pb-doped ZnO nanobelts were prepared by a simply partial cation exchange method, followed by in situ thermal oxidation. Detailed characterization confirmed that Pb was uniformly distributed on porous nanobelts. Additionally, it occupied the Zn situation, not forming its oxides. The gas-sensing measurements revealed that 0.61 at% Pb-doped ZnO porous nanobelts exhibited a selectively enhanced response with long-term stability toward n-butanol among the investigated VOCs. The relative response to 50 ppm of n-butanol was up to 47.7 at the working temperature of 300 °C. Additionally, the response time was short (about 5 s). These results were mainly ascribed to the porous nanostructure, two-dimensional belt-like morphology, enriched oxygen vacancies and the specific synergistic effect from the Pb dopant. Finally, a possible sensing mechanism of porous Pb-doped ZnO nanobelts is proposed and discussed. Full article
(This article belongs to the Special Issue Chemical Sensors for Volatile Organic Compound Detection)
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Article
Voltammetric Determination of Active Pharmaceutical Ingredients Using Screen-Printed Electrodes
Chemosensors 2022, 10(3), 95; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030095 - 01 Mar 2022
Viewed by 912
Abstract
A simple, fast, sensitive and low-cost voltammetric method using a screen-printed carbon electrode (SPCE) is presented in this work for the simultaneous determination of ascorbic acid (AA), paracetamol (PA), dextromethorphan (DX) and caffeine (CF) in both pharmaceutical formulations and samples of environmental interest. [...] Read more.
A simple, fast, sensitive and low-cost voltammetric method using a screen-printed carbon electrode (SPCE) is presented in this work for the simultaneous determination of ascorbic acid (AA), paracetamol (PA), dextromethorphan (DX) and caffeine (CF) in both pharmaceutical formulations and samples of environmental interest. The oxidative peak current displayed linear dependence on concentration within the range 1.7–60.5, 0.6–40.0, 0.9–8.4 (1st linear part) and 1.8–22.0 mg L−1 for AA, PA, DX and CF, respectively; and detection limits of 0.5, 0.2, 0.3 and 0.5 mg L−1, respectively. The developed differential pulse voltammetric (DPV) method was validated using both a pharmaceutical product and a spiked well water sample. A very good agreement between the determined and the theoretical label drug content and recoveries in the range of 99.5–100.8% were obtained for pharmaceutical product and well water samples, respectively. Full article
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Article
An Electrochemical and Raman Scattering Dual Detection Biosensor for Rapid Screening and Biomolecular Profiling of Cancer Biomarkers
Chemosensors 2022, 10(3), 93; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030093 - 28 Feb 2022
Viewed by 843
Abstract
Detecting circulating biomarkers sensitively and quantitatively is paramount for cancer screening, diagnosis, and treatment selection. Particularly, screening of a panel of circulating protein biomarkers followed by mapping of individual biomarkers could assist better diagnosis and understanding of the cancer progression mechanisms. Herein, we [...] Read more.
Detecting circulating biomarkers sensitively and quantitatively is paramount for cancer screening, diagnosis, and treatment selection. Particularly, screening of a panel of circulating protein biomarkers followed by mapping of individual biomarkers could assist better diagnosis and understanding of the cancer progression mechanisms. Herein, we present a miniaturized biosensing platform with dual readout schemes (electrochemical and Surface enhanced Raman scattering (SERS)) for rapid cancer screening and specific biomarker expressional profiling to support cancer management. Our approach utilizes a controlled nanomixing phenomena under alternative current electrohydrodynamic condition to improve the isolation of cancer-associated circulating proteins (i.e., Epidermal growth factor receptor (EGFR), BRAF, Programmed death-ligand 1 (PD-L1)) with antibody functionalized sensor surface for rapid and efficient isolation of the targets and subsequent labelling with SERS nanotags. The method employs Differential Pulse Voltammetry (DPV) for rapidly screening for the presence of the circulating proteins on biosensor surface irrespective of their type. Upon positive DPV detection, SERS is applied for sensitive read-out of individual biomarkers biomarker levels. In a proof-of-concept study, we demonstrate the dual detection biosensor for analysing circulating BRAF, EGFR and PDL-1 proteins and successfully screened both ensemble and individual biomarker expressional levels as low as 10 pg (1 ng/mL). Our findings clearly indicate the potential of the proposed method for cancer biomarker analysis which may drive the translation of this dual sensing concept in clinical settings. Full article
(This article belongs to the Special Issue Quantitative Sensing in the Microspace)
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Article
Sensing Alzheimer’s Disease Utilizing Au Electrode by Controlling Nanorestructuring
Chemosensors 2022, 10(3), 94; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030094 - 27 Feb 2022
Viewed by 1232
Abstract
This paper reports the development of Alzheimer’s disease (AD) sensor through early detection of amyloid-beta (Aβ) (1–42) using simple nanorestructuring of Au sheet plate by oxidation-reduction cycle (ORC) via the electrochemical system. The topology of Au substrates was enhanced through the roughening and [...] Read more.
This paper reports the development of Alzheimer’s disease (AD) sensor through early detection of amyloid-beta (Aβ) (1–42) using simple nanorestructuring of Au sheet plate by oxidation-reduction cycle (ORC) via the electrochemical system. The topology of Au substrates was enhanced through the roughening and Au grains grown by a simple ORC technique in aqueous solutions containing 0.1 mol/L KCl electrolytes. The roughened substrate was then functionalized with the highly specific antibody β-amyloid Aβ (1–28) through HS-PEG-NHS modification, which enabled effective and direct detection of Aβ (1–42) peptide. The efficacy of the ORC method had been exhibited in the polished Au surface by approximately 15% larger electro-active sites compared to the polished Au without ORC. The ORC polished structure demonstrated a rapid, accurate, precise, reproducible, and highly sensitive detection of Aβ (1–42) peptide with a low detection limit of 10.4 fg/mL and a wide linear range of 10−2 to 106 pg/mL. The proposed structure had been proven to have potential as an early-stage Alzheimer’s disease (AD) detection platform with low-cost fabrication and ease of operation. Full article
(This article belongs to the Special Issue Applications of Probe Sensing in Medicine)
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Article
Poly(Thionine)-Modified Screen-Printed Electrodes for CA 19-9 Detection and Its Properties in Raman Spectroscopy
Chemosensors 2022, 10(3), 92; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030092 - 27 Feb 2022
Viewed by 850
Abstract
Polythionine (PTH) is an electroactive compound known for its excellent electron transfer capacity. It has stable and redox centers in its structure, and it can also be generated by electropolymerization of thionine (TH). Due to its properties, it has been used in a [...] Read more.
Polythionine (PTH) is an electroactive compound known for its excellent electron transfer capacity. It has stable and redox centers in its structure, and it can also be generated by electropolymerization of thionine (TH). Due to its properties, it has been used in a large number of applications, including the construction of electrochemical biosensors. In this work, PTH is explored for its ability to generate electrons, which allows it to act as an electrochemical probe in a biosensor that detects CA 19-9 on two different substrates, carbon and gold, using differential pulse voltammetry (DPV) as a reading technique in phosphate buffer (PhB). The analytical features of the resulting electrodes are given, showing linear ranges from 0.010 to 10 U/mL. The Raman spectra of PTH films on gold (substrates or nanostars) and carbon (substrates) are also presented and discussed as a potential use for SERS readings as complementary information to electrochemical data. Full article
(This article belongs to the Special Issue Recent Developments in Platforms for SERS Applications)
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Article
Zinc Donor–Acceptor Schiff Base Complexes as Thermally Activated Delayed Fluorescence Emitters
Chemosensors 2022, 10(3), 91; https://0-doi-org.brum.beds.ac.uk/10.3390/chemosensors10030091 - 26 Feb 2022
Viewed by 1023
Abstract
Four new zinc(II) Schiff base complexes with carbazole electron donor units and either a 2,3-pyrazinedicarbonitrile or a phthalonitrile acceptor unit were synthesized. The donor units are equipped with two bulky 2-ethylhexyl alkyl chains to increase the solubility of the complexes in organic solvents. [...] Read more.
Four new zinc(II) Schiff base complexes with carbazole electron donor units and either a 2,3-pyrazinedicarbonitrile or a phthalonitrile acceptor unit were synthesized. The donor units are equipped with two bulky 2-ethylhexyl alkyl chains to increase the solubility of the complexes in organic solvents. Furthermore, the effect of an additional phenyl linker between donor and acceptor unit on the photophysical properties was investigated. Apart from prompt fluorescence, the Schiff base complexes show thermally activated delayed fluorescence (TADF) with quantum yields up to 47%. The dyes bearing a phthalonitrile acceptor emit in the green–yellow part of the electromagnetic spectrum and those with the stronger 2,3-pyrazinedicarbonitrile acceptor—in the orange–red part of the spectrum. The emission quantum yields decrease upon substitution of phthalonitrile with 2,3-pyrazinedicarbonitrile and upon introduction of the phenyl spacer. The TADF decay times vary between 130 µs and 3.5 ms at ambient temperature. The weaker phthalonitrile acceptor and the additional phenyl linker favor longer TADF decay times. All the complexes show highly temperature-dependent TADF decay time (temperature coefficients above −3%/K at ambient conditions) which makes them potentially suitable for application as molecular thermometers. Immobilized into cell-penetrating RL-100 nanoparticles, the best representative shows temperature coefficients of −5.4%/K at 25 °C that makes the material interesting for further application in intracellular imaging. Full article
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