Research

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14 pages, 4221 KiB

Open AccessArticle

In Situ-Derived N-Doped ZnO from ZIF-8 for Enhanced Ethanol Sensing in ZnO/MEMS Devices

by Meihua Liang, Yong Yan, Jiaxuan Yang, Xiaodong Liu, Rongrong Jia, Yuanyuan Ge, Zhili Li and Lei Huang

Molecules 2024, 29(8), 1703; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules29081703 - 10 Apr 2024

Viewed by 361

Abstract

Microelectromechanical systems (MEMS) gas sensors have numerous advantages such as compact size, low power consumption, ease of integration, etc., while encountering challenges in sensitivity and high resistance because of their low sintering temperature. This work utilizes the in situ growth of Zeolitic Imidazolate [...] Read more.

Microelectromechanical systems (MEMS) gas sensors have numerous advantages such as compact size, low power consumption, ease of integration, etc., while encountering challenges in sensitivity and high resistance because of their low sintering temperature. This work utilizes the in situ growth of Zeolitic Imidazolate Framework-8 (ZIF-8) followed by its conversion to N-doped ZnO. The results obtained from scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicate that the in situ derivation of ZIF-8 facilitates the adhesion of ZnO particles, forming an island-like structure and significantly reducing the interfaces between these particles. Furthermore, powder X-ray diffraction (XRD) analysis, elemental mapping, and X-ray photoelectron spectroscopy (XPS) analysis confirm the conversion of ZIF-8 to ZnO, the successful incorporation of N atoms into the ZnO lattice, and the creation of more oxygen vacancies. The ZIF-8-derived N-doped ZnO/MEMS sensor (ZIF (3)-ZnO/MEMS) exhibits remarkable gas sensitivity for ethanol detection. At an operating temperature of 290 °C, it delivers a substantial response value of 80 towards 25 ppm ethanol, a 13-fold enhancement compared with pristine ZnO/MEMS sensors. The sensor also exhibits an ultra-low theoretical detection limit of 11.5 ppb to ethanol, showcasing its excellent selectivity. The enhanced performance is attributed to the incorporation of N-doped ZnO, which generates abundant oxygen vacancies on the sensor’s surface, leading to enhanced interaction with ethanol molecules. Additionally, a substantial two-order-of-magnitude decrease in the resistance of the gas-sensitive film is observed. Overall, this study provides valuable insights into the design and fabrication strategies applicable to high-performance MEMS gas sensors in a broader range of gas sensing. Full article

(This article belongs to the Special Issue Nano-Functional Materials for Sensor Applications)

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14 pages, 1744 KiB

Open AccessArticle

Catalase Detection via Membrane-Based Pressure Sensors

by Monica Bianco, Alessandra Zizzari, Elisabetta Perrone, Diego Mangiullo, Marco Mazzeo, Ilenia Viola and Valentina Arima

Molecules 2024, 29(7), 1506; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules29071506 - 28 Mar 2024

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Abstract

Membrane-based sensors (MePSs) exhibit remarkable precision and sensitivity in detecting pressure changes. MePSs are commonly used to monitor catalytic reactions in solution, generating gas products crucial for signal amplification in bioassays. They also allow for catalyst quantification by indirectly measuring the pressure generated [...] Read more.

Membrane-based sensors (MePSs) exhibit remarkable precision and sensitivity in detecting pressure changes. MePSs are commonly used to monitor catalytic reactions in solution, generating gas products crucial for signal amplification in bioassays. They also allow for catalyst quantification by indirectly measuring the pressure generated by the gaseous products. This is particularly interesting for detecting enzymes in biofluids associated with disease onset. To enhance the performance of a MePS, various structural factors influence membrane flexibility and response time, ultimately dictating the device’s pressure sensitivity. In this study, we fabricated MePSs using polydimethylsiloxane (PDMS) and investigated how structural modifications affect the Young’s modulus (E) and residual stress (σ₀) of the membranes. These modifications have a direct impact on the sensors’ sensitivity to pressure variations, observed as a function of the volume of the chamber (Σ) or of the mechanical properties of the membrane itself (S). MePSs exhibiting the highest sensitivities were then employed to detect catalyst quantities inducing the dismutation of hydrogen peroxide, producing dioxygen as a gaseous product. As a result, a catalase enzyme was successfully detected using these optimized MePSs, achieving a remarkable sensitivity of (22.7 ± 1.2) µm/nM and a limit of detection (LoD) of 396 pM. Full article

(This article belongs to the Special Issue Nano-Functional Materials for Sensor Applications)

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13 pages, 4690 KiB

Open AccessArticle

Silver Nanoparticle-Embedded Hydrogels for Electrochemical Sensing of Sulfamethoxazole Residues in Meat

by Yuanxi Deng and Ningning Yang

Molecules 2024, 29(6), 1256; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules29061256 - 12 Mar 2024

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Abstract

A disposable electrochemical sensor based on silver nanoparticle-embedded cellulose hydrogel composites was developed for sensitive detection of sulfamethoxazole residues in meat samples. Scanning electron microscopy confirmed the porous structure of the cellulose matrix anchored with 20–50 nm silver nanoparticles (AgNPs). Fourier transform infrared [...] Read more.

A disposable electrochemical sensor based on silver nanoparticle-embedded cellulose hydrogel composites was developed for sensitive detection of sulfamethoxazole residues in meat samples. Scanning electron microscopy confirmed the porous structure of the cellulose matrix anchored with 20–50 nm silver nanoparticles (AgNPs). Fourier transform infrared spectroscopy and X-ray diffraction verified that the metallic AgNPs coordinated with the amorphous cellulose chains. At an optimum 0.5% loading, the nanocomposite sensor showed a peak-to-peak separation of 150 mV, diffusion-controlled charge transfer kinetics, and an electron transfer coefficient of 0.6 using a ferro/ferricyanide redox probe. Square-wave voltammetry was applied for sensing sulfamethoxazole based on its two-electron oxidation peak at 0.72 V vs. Ag/AgCl in Britton–Robinson buffer of pH 7.0. A linear detection range of 0.1–100 μM sulfamethoxazole was obtained with a sensitivity of 0.752 μA/μM and limit of detection of 0.04 μM. Successful recovery between 86 and 92% and less than 6% RSD was achieved from spiked meat samples. The key benefits of the proposed disposable sensor include facile fabrication, an antifouling surface, and a reliable quantification ability, meeting regulatory limits. This research demonstrates the potential of novel cellulose–silver nanocomposite materials towards developing rapid, low-cost electroanalytical devices for decentralized on-site screening of veterinary drug residues to ensure food safety. Full article

(This article belongs to the Special Issue Nano-Functional Materials for Sensor Applications)

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12 pages, 2805 KiB

Open AccessArticle

Rapid Detection of the Anti-Tumor Drug Etoposide in Biological Samples by Using a Nanoporous-Gold-Based Electrochemical Sensor

by Huiyuan Yu, Mengjie Hu, Xiaolei Wang, Xia Wang, Luying Xun and Honglei Liu

Molecules 2024, 29(5), 1060; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules29051060 - 28 Feb 2024

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Abstract

Monitoring etoposide is important due to its wide usage in anti-tumor therapy; however, the commonly used HPLC method is expensive and often requires complicated extraction and detection procedures. Electrochemical analysis has great application prospects because of its rapid response and high specificity, sensitivity, [...] Read more.

Monitoring etoposide is important due to its wide usage in anti-tumor therapy; however, the commonly used HPLC method is expensive and often requires complicated extraction and detection procedures. Electrochemical analysis has great application prospects because of its rapid response and high specificity, sensitivity, and efficiency with low cost and high convenience. In this study, we constructed a nanoporous gold (NPG)-modified GCE for the detection of etoposide. The electrochemical oxidation of etoposide by NPG caused a sensitive current peak at +0.27 V with good reproductivity in 50 mM of phosphate buffer (pH 7.4). The relationship between etoposide concentration and peak current was linear in the range between 0.1 and 20 μM and between 20 and 150 μM, with a detection sensitivity of 681.8 μA mM⁻¹ cm⁻² and 197.2 μA mM⁻¹ cm⁻², respectively, and a limit of detection (LOD) reaching 20 nM. The electrode had a good anti-interference ability to several common anions and cations. Spiked recovery tests in serum, urine, and fermentation broth verified the excellent performance of the sensor in terms of sensitivity, reproducibility, and specificity. This may provide a promising tool for the detection of etoposide in biological samples. Full article

(This article belongs to the Special Issue Nano-Functional Materials for Sensor Applications)

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11 pages, 1352 KiB

Open AccessArticle

Changes in the Main Physicochemical Properties and Electrochemical Fingerprints in the Production of Sea Buckthorn Juice by Pectinase Treatment

by Kaihua Guo

Molecules 2024, 29(5), 1035; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules29051035 - 28 Feb 2024

Viewed by 510

Abstract

Enzymatic hydrolysis using pectinase is critical for producing high-yield and quality sea buckthorn juice. This study determined the optimal temperature, time, and enzyme dosage combinations to guide manufacturers. A temperature of 60 °C, hydrolysis time of 3 h, and 0.3% enzyme dosage gave [...] Read more.

Enzymatic hydrolysis using pectinase is critical for producing high-yield and quality sea buckthorn juice. This study determined the optimal temperature, time, and enzyme dosage combinations to guide manufacturers. A temperature of 60 °C, hydrolysis time of 3 h, and 0.3% enzyme dosage gave 64.1% juice yield—25% higher than without enzymes. Furthermore, monitoring physicochemical properties reveals enzyme impacts on composition. Higher dosages increase soluble solids up to 15% and soluble fiber content by 35% through cell wall breakdown. However, excessive amounts over 0.3% decrease yields. Pectin concentration also declines dose-dependently, falling by 91% at 0.4%, improving juice stability but needing modulation to retain viscosity. Electrochemical fingerprinting successfully differentiates process conditions, offering a rapid quality control tool. Its potential for commercial inline use during enzymatic treatment requires exploration. Overall, connecting optimized parameters to measured effects provides actionable insights for manufacturers to boost yields, determine enzyme impacts on nutrition/functionality, and introduce novel process analytical technology. Further investigations of health properties using these conditions could expand sea buckthorn juice functionality. Full article

(This article belongs to the Special Issue Nano-Functional Materials for Sensor Applications)

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11 pages, 2622 KiB

Open AccessArticle

Preparation of β-Cyclodextrin Functionalized Platform for Monitoring Changes in Potassium Content in Perspiration

by Ruixiang Liu and Xiaofeng Shi

Molecules 2023, 28(19), 7000; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28197000 - 09 Oct 2023

Viewed by 825

Abstract

The monitoring of potassium ion (K⁺) levels in human sweat can provide valuable insights into electrolyte balance and muscle fatigue non-invasively. However, existing laboratory techniques for sweat testing are complex, while wearable sensors face limitations like drift, fouling and interference from [...] Read more.

The monitoring of potassium ion (K⁺) levels in human sweat can provide valuable insights into electrolyte balance and muscle fatigue non-invasively. However, existing laboratory techniques for sweat testing are complex, while wearable sensors face limitations like drift, fouling and interference from ions such as Na⁺. This work develops printed electrodes using β-cyclodextrin functionalized reduced graphene oxide (β-CD-RGO) for selective K⁺ quantification in sweat. The β-CD prevents the aggregation of RGO sheets while also providing selective binding sites for K⁺ capture. Electrodes were fabricated by screen printing the β-CD-RGO ink onto conductive carbon substrates. Material characterization confirmed the successful functionalization of RGO with β-CD. Cyclic voltammetry (CV) showed enhanced electrochemical behavior for β-CD-RGO-printed electrodes compared with bare carbon and RGO. Sensor optimization resulted in a formulation with 30% β-CD-RGO loading. The printed electrodes were drop-casted with an ion-selective polyvinyl chloride (PVC) membrane. A linear range from 10 μM to 100 mM was obtained along with a sensitivity of 54.7 mV/decade. The sensor showed good reproducibility over 10 cycles in 10 mM KCl. Minimal interference from 100 mM Na⁺ and other common sweat constituents validated the sensor’s selectivity. On-body trials were performed by mounting the printed electrodes on human subjects during exercise. The K⁺ levels measured in sweat were found to correlate well with serum analysis, demonstrating the sensor’s ability for non-invasive electrolyte monitoring. Overall, the facile synthesis of stable β-CD-RGO inks enables the scalable fabrication of wearable sensors for sweat potassium detection. Full article

(This article belongs to the Special Issue Nano-Functional Materials for Sensor Applications)

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10 pages, 2011 KiB

Open AccessArticle

Fabry–Pérot Cavities with Suspended Palladium Membranes on Optical Fibers for Highly Sensitive Hydrogen Sensing

by Feng Xu, Jun Ma, Can Li, Churong Ma, Jie Li, Bai-Ou Guan and Kai Chen

Molecules 2023, 28(19), 6984; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28196984 - 09 Oct 2023

Cited by 1 | Viewed by 870

Abstract

Hydrogen (H₂) sensors are critical to various applications such as the situation where H₂ is used as the clean energy for industry or the indicator for human disease diagnosis. Palladium (Pd) is widely used as the hydrogen sensing material in [...] Read more.

Hydrogen (H₂) sensors are critical to various applications such as the situation where H₂ is used as the clean energy for industry or the indicator for human disease diagnosis. Palladium (Pd) is widely used as the hydrogen sensing material in different types of sensors. Optical fiber H₂ sensors are particularly promising due to their compactness and spark-free operation. Here, we report a Fabry–Pérot (FP)-cavity-based H₂ sensor that is formed with a freestanding Pd membrane and integrated on a conventional single-mode optical fiber end. The freestanding Pd membrane acts both as the active hydrogen sensing material and as one of the reflective mirrors of the cavity. When the Pd film absorbs H₂ to form PdH_x, it will be stretched, resulting in a change of the cavity length and thus a shift of the interference spectrum. The H₂ concentration can be derived from the amplitude of the wavelength shift. Experimental results showed that H₂ sensors based on suspended Pd membranes can achieve a detection sensitivity of about 3.6 pm/ppm and a detection limit of about 3.3 ppm. This highly sensitive detection scheme is expected to find applications for sensing low-concentration H₂. Full article

(This article belongs to the Special Issue Nano-Functional Materials for Sensor Applications)

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Review

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25 pages, 3980 KiB

Open AccessReview

A Review of Recent Progress in Drug Doping and Gene Doping Control Analysis

by Yuze Lu, Jiayu Yan, Gaozhi Ou and Li Fu

Molecules 2023, 28(14), 5483; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28145483 - 18 Jul 2023

Cited by 4 | Viewed by 2396

Abstract

The illicit utilization of performance-enhancing substances, commonly referred to as doping, not only infringes upon the principles of fair competition within athletic pursuits but also poses significant health hazards to athletes. Doping control analysis has emerged as a conventional approach to ensuring equity [...] Read more.

The illicit utilization of performance-enhancing substances, commonly referred to as doping, not only infringes upon the principles of fair competition within athletic pursuits but also poses significant health hazards to athletes. Doping control analysis has emerged as a conventional approach to ensuring equity and integrity in sports. Over the past few decades, extensive advancements have been made in doping control analysis methods, catering to the escalating need for qualitative and quantitative analysis of numerous banned substances exhibiting diverse chemical and biological characteristics. Progress in science, technology, and instrumentation has facilitated the proliferation of varied techniques for detecting doping. In this comprehensive review, we present a succinct overview of recent research developments within the last ten years pertaining to these doping detection methodologies. We undertake a comparative analysis, evaluating the merits and limitations of each technique, and offer insights into the prospective future advancements in doping detection methods. It is noteworthy that the continual design and synthesis of novel synthetic doping agents have compelled researchers to constantly refine and innovate doping detection methods in order to address the ever-expanding range of covertly employed doping agents. Overall, we remain in a passive position for doping detection and are always on the road to doping control. Full article

(This article belongs to the Special Issue Nano-Functional Materials for Sensor Applications)

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