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Keywords = surface-enhanced Raman spectrometry

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46 pages, 3177 KiB  
Review
Recent Advancements in Lateral Flow Assays for Food Mycotoxin Detection: A Review of Nanoparticle-Based Methods and Innovations
by Gayathree Thenuwara, Perveen Akhtar, Bilal Javed, Baljit Singh, Hugh J. Byrne and Furong Tian
Toxins 2025, 17(7), 348; https://doi.org/10.3390/toxins17070348 - 11 Jul 2025
Viewed by 626
Abstract
Mycotoxins are responsible for a multitude of diseases in both humans and animals, resulting in significant medical and economic burdens worldwide. Conventional detection methods, such as enzyme-linked immunosorbent assay (ELISA), high-performance liquid chromatography (HPLC), and liquid chromatography-tandem mass spectrometry (LC-MS/MS), are highly effective, [...] Read more.
Mycotoxins are responsible for a multitude of diseases in both humans and animals, resulting in significant medical and economic burdens worldwide. Conventional detection methods, such as enzyme-linked immunosorbent assay (ELISA), high-performance liquid chromatography (HPLC), and liquid chromatography-tandem mass spectrometry (LC-MS/MS), are highly effective, but they are generally confined to laboratory settings. Consequently, there is a growing demand for point-of-care testing (POCT) solutions that are rapid, sensitive, portable, and cost-effective. Lateral flow assays (LFAs) are a pivotal technology in POCT due to their simplicity, rapidity, and ease of use. This review synthesizes data from 78 peer-reviewed studies published between 2015 and 2024, evaluating advances in nanoparticle-based LFAs for detection of singular or multiplex mycotoxin types. Gold nanoparticles (AuNPs) remain the most widely used, due to their favorable optical and surface chemistry; however, significant progress has also been made with silver nanoparticles (AgNPs), magnetic nanoparticles, quantum dots (QDs), nanozymes, and hybrid nanostructures. The integration of multifunctional nanomaterials has enhanced assay sensitivity, specificity, and operational usability, with innovations including smartphone-based readers, signal amplification strategies, and supplementary technologies such as surface-enhanced Raman spectroscopy (SERS). While most singular LFAs achieved moderate sensitivity (0.001–1 ng/mL), only 6% reached ultra-sensitive detection (<0.001 ng/mL), and no significant improvement was evident over time (ρ = −0.162, p = 0.261). In contrast, multiplex assays demonstrated clear performance gains post-2022 (ρ = −0.357, p = 0.0008), largely driven by system-level optimization and advanced nanomaterials. Importantly, the type of sample matrix (e.g., cereals, dairy, feed) did not significantly influence the analytical sensitivity of singular or multiplex lateral LFAs (Kruskal–Wallis p > 0.05), confirming the matrix-independence of these optimized platforms. While analytical challenges remain for complex targets like fumonisins and deoxynivalenol (DON), ongoing innovations in signal amplification, biorecognition chemistry, and assay standardization are driving LFAs toward becoming reliable, ultra-sensitive, and field-deployable platforms for high-throughput mycotoxin screening in global food safety surveillance. Full article
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18 pages, 3348 KiB  
Article
Moderate-Temperature Pyrolysis Characteristics of Lump Coal Under Varying Coal Particle Sizes
by Yuanpei Luo, Luxuan Liu, Liangguo Lv, Shengping Zhang, Fei Dai, Hongguang Jin and Jun Sui
Energies 2025, 18(12), 3220; https://doi.org/10.3390/en18123220 - 19 Jun 2025
Viewed by 381
Abstract
Pyrolysis is an important methodology for achieving efficient and clean utilization of coal. Lump coal pyrolysis demonstrates distinct advantages over pulverized coal processing, particularly in enhanced gas yield and superior coke quality. As a critical parameter in lump coal pyrolysis, particle size significantly [...] Read more.
Pyrolysis is an important methodology for achieving efficient and clean utilization of coal. Lump coal pyrolysis demonstrates distinct advantages over pulverized coal processing, particularly in enhanced gas yield and superior coke quality. As a critical parameter in lump coal pyrolysis, particle size significantly influences heat transfer and mass transfer during pyrolysis, yet its governing mechanisms remain insufficiently explored. This research systematically investigates pyrolysis characteristics of the low-rank coal from Ordos, Inner Mongolia, across graded particle sizes (2–5 mm, 5–10 mm, 10–20 mm, and 20–30 mm) through pyrolysis experiments. Real-time central temperature monitoring of coal bed coupled with advanced characterization techniques—including X-ray diffraction (XRD), Raman spectroscopy, Brunauer–Emmett–Teller (BET) analysis, scanning electron microscopy (SEM), gas chromatography (GC), and GC–mass spectrometry (GC-MS)—reveals particle-size-dependent pyrolysis mechanisms. Key findings demonstrate that the larger particles enhance bed-scale convective heat transfer, accelerating temperature propagation from reactor walls to the coal center. However, excessive sizes cause significant intra-particle thermal gradients, impeding core pyrolysis. The 10–20 mm group emerges as optimal—balancing these effects to achieve uniform thermal attainment, evidenced by 20.99 vol% peak hydrogen yield and maximum char graphitization. Tar yield first demonstrates a tendency to rise and then decline, peaking at 14.66 wt.% for 5–10 mm particles. This behavior reflects competing mechanisms: enlarging particle size can improve bed permeability (reducing tar residence time and secondary reactions), but it can also inhibit volatile release and intensify thermal cracking of tar in oversized coal blocks. The BET analysis result reveals elevated specific surface area and pore volume with increasing particle size, except for the 10–20 mm group, showing abrupt porosity reduction—attributed to pore collapse caused by intense polycondensation reactions. Contrasting previous studies predominantly focused on less than 2 mm pulverized coal, this research selects large-size (from 2 mm to 30 mm) lump coal to clarify the effect of particle size on coal pyrolysis, providing critical guidance for industrial-scale lump coal pyrolysis optimization. Full article
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28 pages, 3203 KiB  
Article
From Pollutant Removal to Renewable Energy: MoS2-Enhanced P25-Graphene Photocatalysts for Malathion Degradation and H2 Evolution
by Cristian Martínez-Perales, Abniel Machín, Pedro J. Berríos-Rolón, Paola Sampayo, Enrique Nieves, Loraine Soto-Vázquez, Edgard Resto, Carmen Morant, José Ducongé, María C. Cotto and Francisco Márquez
Materials 2025, 18(11), 2602; https://doi.org/10.3390/ma18112602 - 3 Jun 2025
Viewed by 1097
Abstract
The widespread presence of pesticides—especially malathion—in aquatic environments presents a major obstacle to conventional remediation strategies, while the ongoing global energy crisis underscores the urgency of developing renewable energy sources such as hydrogen. In this context, photocatalytic water splitting emerges as a promising [...] Read more.
The widespread presence of pesticides—especially malathion—in aquatic environments presents a major obstacle to conventional remediation strategies, while the ongoing global energy crisis underscores the urgency of developing renewable energy sources such as hydrogen. In this context, photocatalytic water splitting emerges as a promising approach, though its practical application remains limited by poor charge carrier dynamics and insufficient visible-light utilization. Herein, we report the design and evaluation of a series of TiO2-based ternary nanocomposites comprising commercial P25 TiO2, reduced graphene oxide (rGO), and molybdenum disulfide (MoS2), with MoS2 loadings ranging from 1% to 10% by weight. The photocatalysts were fabricated via a two-step method: hydrothermal integration of rGO into P25 followed by solution-phase self-assembly of exfoliated MoS2 nanosheets. The composites were systematically characterized using X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectroscopy (DRS), and photoluminescence (PL) spectroscopy. Photocatalytic activity was assessed through two key applications: the degradation of malathion (20 mg/L) under simulated solar irradiation and hydrogen evolution from water in the presence of sacrificial agents. Quantification was performed using UV-Vis spectroscopy, gas chromatography–mass spectrometry (GC-MS), and thermal conductivity detection (GC-TCD). Results showed that the integration of rGO significantly enhanced surface area and charge mobility, while MoS2 served as an effective co-catalyst, promoting interfacial charge separation and acting as an active site for hydrogen evolution. Nearly complete malathion degradation (~100%) was achieved within two hours, and hydrogen production reached up to 6000 µmol g−1 h−1 under optimal MoS2 loading. Notably, photocatalytic performance declined with higher MoS2 content due to recombination effects. Overall, this work demonstrates the synergistic enhancement provided by rGO and MoS2 in a stable P25-based system and underscores the viability of such ternary nanocomposites for addressing both environmental remediation and sustainable energy conversion challenges. Full article
(This article belongs to the Special Issue Catalysis: Where We Are and Where We Go)
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27 pages, 6942 KiB  
Review
Advances in Multifunctional Nanoagents and SERS-Based Multimodal Sensing for Biotoxin in Foods
by Huan Jiang, Sihang Zhang, Bei Li and Long Wu
Foods 2025, 14(8), 1393; https://doi.org/10.3390/foods14081393 - 17 Apr 2025
Viewed by 633
Abstract
Biotoxins, toxic substances produced by living organisms, are widely present in food and pose a major threat to human health. Traditional detection methods, such as gas chromatography-mass spectrometry (GC-MS) and enzyme-linked immunosorbent assay (ELISA), often suffer from limitations including complex sample preparation, high [...] Read more.
Biotoxins, toxic substances produced by living organisms, are widely present in food and pose a major threat to human health. Traditional detection methods, such as gas chromatography-mass spectrometry (GC-MS) and enzyme-linked immunosorbent assay (ELISA), often suffer from limitations including complex sample preparation, high costs, and lengthy analysis times. In response, surface-enhanced Raman spectroscopy (SERS) has emerged as a highly sensitive and specific analytical tool for the detection of biotoxins. This review highlights the recent progress in multimodal detection technologies based on SERS, focusing on the design and classification of multimodal materials to optimize the construction of SERS substrates. The integration of SERS with other detection modalities, such as fluorescence, colorimetry, and electrochemistry, is discussed to enhance the accuracy and diversity of biotoxin detection. Finally, the review critically assesses the current challenges and future prospects of SERS multimodal detection technology, particularly in real-time food safety monitoring and on-site diagnostics, offering critical insights to guide future research directions. Full article
(This article belongs to the Section Food Analytical Methods)
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16 pages, 2959 KiB  
Article
Efficacy of Household and Commercial Washing Agents in Removing the Pesticide Thiabendazole Residues from Fruits
by Xinyi Du, Lauren Ho, Sisheng Li, Jeffery Doherty, Junghak Lee, John M. Clark and Lili He
Foods 2025, 14(2), 318; https://doi.org/10.3390/foods14020318 - 18 Jan 2025
Cited by 1 | Viewed by 5176
Abstract
Pesticide residues on fruits pose a global food safety concern, emphasizing the need for effective and practical removal strategies to ensure safe consumption. This study investigates the efficacy of household ingredients (corn starch, all-purpose flour, rice flour and baking soda) and four commercial [...] Read more.
Pesticide residues on fruits pose a global food safety concern, emphasizing the need for effective and practical removal strategies to ensure safe consumption. This study investigates the efficacy of household ingredients (corn starch, all-purpose flour, rice flour and baking soda) and four commercial fresh produce wash products in eliminating a model pesticide thiabendazole with and without a model non-ionic surfactant Alligare 90® from postharvest fruits. Surface-enhanced Raman spectroscopy (SERS) was employed for the rapid, in situ quantification of residue removal on apple surfaces. Soaking in 2% corn starch followed by soaking in 5% baking was the most effective homemade strategy, removing 94.13% and 91.78% of thiabendazole with and without the surfactant. Among commercial washing agents, soaking in 2% Product 4 demonstrated the highest efficiency, removing 95.3% and 95.99% of thiabendazole with and without surfactant. These results suggested that the non-ionic surfactant did not affect removal efficiency. Both protocols were effective across various fruits (apples, grapes, lemons, strawberries), validated by liquid chromatography–mass spectrometry (LC-MS/MS) analyses. However, safety concerns regarding the composition of Product 4 highlighted the benefits of homemade strategies. Overall, this work offers practical guidelines for reducing pesticide residues on fruits and enhancing food. Full article
(This article belongs to the Section Food Toxicology)
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36 pages, 1986 KiB  
Review
Exploring Innovative Approaches for the Analysis of Micro- and Nanoplastics: Breakthroughs in (Bio)Sensing Techniques
by Denise Margarita Rivera-Rivera, Gabriela Elizabeth Quintanilla-Villanueva, Donato Luna-Moreno, Araceli Sánchez-Álvarez, José Manuel Rodríguez-Delgado, Erika Iveth Cedillo-González, Garima Kaushik, Juan Francisco Villarreal-Chiu and Melissa Marlene Rodríguez-Delgado
Biosensors 2025, 15(1), 44; https://doi.org/10.3390/bios15010044 - 13 Jan 2025
Cited by 10 | Viewed by 3951
Abstract
Plastic pollution, particularly from microplastics (MPs) and nanoplastics (NPs), has become a critical environmental and health concern due to their widespread distribution, persistence, and potential toxicity. MPs and NPs originate from primary sources, such as cosmetic microspheres or synthetic fibers, and secondary fragmentation [...] Read more.
Plastic pollution, particularly from microplastics (MPs) and nanoplastics (NPs), has become a critical environmental and health concern due to their widespread distribution, persistence, and potential toxicity. MPs and NPs originate from primary sources, such as cosmetic microspheres or synthetic fibers, and secondary fragmentation of larger plastics through environmental degradation. These particles, typically less than 5 mm, are found globally, from deep seabeds to human tissues, and are known to adsorb and release harmful pollutants, exacerbating ecological and health risks. Effective detection and quantification of MPs and NPs are essential for understanding and mitigating their impacts. Current analytical methods include physical and chemical techniques. Physical methods, such as optical and electron microscopy, provide morphological details but often lack specificity and are time-intensive. Chemical analyses, such as Fourier transform infrared (FTIR) and Raman spectroscopy, offer molecular specificity but face challenges with smaller particle sizes and complex matrices. Thermal analytical methods, including pyrolysis gas chromatography–mass spectrometry (Py-GC-MS), provide compositional insights but are destructive and limited in morphological analysis. Emerging (bio)sensing technologies show promise in addressing these challenges. Electrochemical biosensors offer cost-effective, portable, and sensitive platforms, leveraging principles such as voltammetry and impedance to detect MPs and their adsorbed pollutants. Plasmonic techniques, including surface plasmon resonance (SPR) and surface-enhanced Raman spectroscopy (SERS), provide high sensitivity and specificity through nanostructure-enhanced detection. Fluorescent biosensors utilizing microbial or enzymatic elements enable the real-time monitoring of plastic degradation products, such as terephthalic acid from polyethylene terephthalate (PET). Advancements in these innovative approaches pave the way for more accurate, scalable, and environmentally compatible detection solutions, contributing to improved monitoring and remediation strategies. This review highlights the potential of biosensors as advanced analytical methods, including a section on prospects that address the challenges that could lead to significant advancements in environmental monitoring, highlighting the necessity of testing the new sensing developments under real conditions (composition/matrix of the samples), which are often overlooked, as well as the study of peptides as a novel recognition element in microplastic sensing. Full article
(This article belongs to the Special Issue Micro-nano Optic-Based Biosensing Technology and Strategy)
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17 pages, 29213 KiB  
Article
Lubrication-Enhanced Mechanisms of Bentonite Grease Using 2D MoS2 with Narrow Lateral Size and Thickness Distributions
by Shaoyicheng Zhu, Shuo Xiang, Xue Yang, Xin Yang, Hebin Bao, Hao He, Xin Du, Qinhui Zhang, Junjie Zhang, Kai Ma, Yi Cao, Yuehao Liu, Liangyi Peng, Zhitao Li and Yunhong Fan
Lubricants 2024, 12(12), 447; https://doi.org/10.3390/lubricants12120447 - 16 Dec 2024
Viewed by 1195
Abstract
2D MoS2 with narrow lateral size and thickness distributions was introduced to promote the anti-friction and anti-wear properties of the bentonite grease (BG) in a state of boundary lubrication. Optical microscopy (OM), and 3D optical profilers (3D OP), Raman spectrometry (Raman), scanning [...] Read more.
2D MoS2 with narrow lateral size and thickness distributions was introduced to promote the anti-friction and anti-wear properties of the bentonite grease (BG) in a state of boundary lubrication. Optical microscopy (OM), and 3D optical profilers (3D OP), Raman spectrometry (Raman), scanning electron microscope, energy dispersion spectrum (SEM-EDS), and X-ray photoelectron spectroscopy (XPS) were applied to characterize the wear surface of the GCr15 bearing steel/GCr15 bearing steel contact. It is found that the average friction coefficient (AFC), wear scar diameter (WSD), surface roughness and average wear scar depth of BG + 1.2 wt.% 2D MoS2 were effectively reduced by approximately 22.15%, 23.14%, 55.15%, and 21.1%, respectilvely, compared with BG under the working condition of 392N, 75 °C, 1 h, and 1200 rpm. Raman, EDS and XPS results jointly demonstrated that a stable adsorbed film and a robust tribochemical film composed of Fe2O3, FeSO4, Fe2(SO4)3, FeSO3, FeS, FeO and MoO3, which further contributes to the enhancement of lubrication performance. Full article
(This article belongs to the Special Issue Wear-Resistant Coatings and Film Materials)
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16 pages, 3946 KiB  
Article
Effect of Pyrolysis Temperature on the Carbon Sequestration Capacity of Spent Mushroom Substrate Biochar in the Presence of Mineral Iron
by Bin Liu, Zebing Xing, Yuxin Xue, Ji Zhang and Junlin Zhai
Molecules 2024, 29(23), 5712; https://doi.org/10.3390/molecules29235712 - 3 Dec 2024
Viewed by 1999
Abstract
The preparation of biochar typically involves the pyrolysis of waste organic biomass. Iron-rich magnetic biochar not only inherits the characteristics of high specific surface area and porous structure from biochar but also possesses significant advantages in easy separation and recovery, which has shown [...] Read more.
The preparation of biochar typically involves the pyrolysis of waste organic biomass. Iron-rich magnetic biochar not only inherits the characteristics of high specific surface area and porous structure from biochar but also possesses significant advantages in easy separation and recovery, which has shown great application potential in various fields such as soil improvement and water resource remediation. This study aims to explore the influence of mineral iron on the carbon sequestration capability of biochar during the pyrolysis process. Experiments were conducted by using spent mushroom substrates as raw materials to prepare biochar at different temperature intervals (300 to 600 °C). The addition of exogenous iron has been found to significantly enhance the carbon retention rate (12.2–44.5%) of biochar across various pyrolysis temperatures and, notably, improves the carbon stability of biochar at 300 °C, 400 °C, and 600 °C. Through the analysis of thermogravimetric mass spectrometry (TG-MS) and X-ray photoelectron spectroscopy (XPS), we discovered that iron catalyzes the thermochemical reactions and inhibits the release of organic small molecules (C2-C5) through both physical blocking (FexOx) and chemical bonding (C=O and O-C=O). The results of Raman spectroscopy and infrared spectroscopy analyses indicate that the addition of iron significantly promotes the graphitization process of carbon and enhances the thermal stability of biochar within the temperature range of 300 to 500 °C. When exploring the retention and stability of carbon during pyrolysis, it was found that under the conditions of 600 °C and the presence of iron, the maximum carbon sequestration rate of biochar can reach 60.6%. Overall, this study highlights the critical role of iron and pyrolysis temperature in enhancing the carbon sequestration capacity of biochar. Full article
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25 pages, 5952 KiB  
Review
The Evolution of Illicit-Drug Detection: From Conventional Approaches to Cutting-Edge Immunosensors—A Comprehensive Review
by Nigar Anzar, Shariq Suleman, Yashda Singh, Supriya Kumari, Suhel Parvez, Roberto Pilloton and Jagriti Narang
Biosensors 2024, 14(10), 477; https://doi.org/10.3390/bios14100477 - 3 Oct 2024
Cited by 5 | Viewed by 3236
Abstract
The increasing use of illicit drugs has become a major global concern. Illicit drugs interact with the brain and the body altering an individual’s mood and behavior. As the substance-of-abuse (SOA) crisis continues to spread across the world, in order to reduce trafficking [...] Read more.
The increasing use of illicit drugs has become a major global concern. Illicit drugs interact with the brain and the body altering an individual’s mood and behavior. As the substance-of-abuse (SOA) crisis continues to spread across the world, in order to reduce trafficking and unlawful activity, it is important to use point-of-care devices like biosensors. Currently, there are certain conventional detection methods, which include gas chromatography (GC), mass spectrometry (MS), surface ionization, surface-enhanced Raman spectroscopy (SERS), surface plasmon resonance (SPR), electrochemiluminescence (ECL), high-performance liquid chromatography (HPLC), etc., for the detection of abused drugs. These methods have the advantage of high accuracy and sensitivity but are generally laborious, expensive, and require trained operators, along with high sample requirements, and they are not suitable for on-site drug detection scenarios. As a result, there is an urgent need for point-of-care technologies for a variety of drugs that can replace conventional techniques, such as a biosensor, specifically an immunosensor. An immunosensor is an analytical device that integrates an antibody-based recognition element with a transducer to detect specific molecules (antigens). In an immunosensor, the highly selective antigen–antibody interaction is used to identify and quantify the target analyte. The binding event between the antibody and antigen is converted by the transducer into a measurable signal, such as electrical, optical, or electrochemical, which corresponds to the presence and concentration of the analyte in the sample. This paper provides a comprehensive overview of various illicit drugs, the conventional methods employed for their detection, and the advantages of immunosensors over conventional techniques. It highlights the critical need for on-site detection and explores emerging point-of-care testing methods. The paper also outlines future research goals in this field, emphasizing the potential of advanced technologies to enhance the accuracy, efficiency, and convenience of drug detection. Full article
(This article belongs to the Special Issue Feature Paper in Biosensor and Bioelectronic Devices 2024)
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15 pages, 2780 KiB  
Article
Enhanced Sensitivity and Homogeneity of SERS Signals on Plasmonic Substrate When Coupled to Paper Spray Ionization–Mass Spectrometry
by Adewale A. Adehinmoye, Ebenezer H. Bondzie, Jeremy D. Driskell, Christopher C. Mulligan and Jun-Hyun Kim
Chemosensors 2024, 12(9), 175; https://doi.org/10.3390/chemosensors12090175 - 2 Sep 2024
Cited by 1 | Viewed by 2016
Abstract
This work reports on the development of an analyte sampling strategy on a plasmonic substrate to amplify the detection capability of a dual analytical system, paper spray ionization–mass spectrometry (PSI-MS) and surface-enhanced Raman spectroscopy (SERS). While simply applying only an analyte solution to [...] Read more.
This work reports on the development of an analyte sampling strategy on a plasmonic substrate to amplify the detection capability of a dual analytical system, paper spray ionization–mass spectrometry (PSI-MS) and surface-enhanced Raman spectroscopy (SERS). While simply applying only an analyte solution to the plasmonic paper results in a limited degree of SERS enhancement, the introduction of plasmonic gold nanoparticles (AuNPs) greatly improves the SERS signals without sacrificing PSI-MS sensitivity. It is initially revealed that the concentration of AuNPs and the type of analytes highly influence the SERS signals and their variations due to the “coffee ring effect” flow mechanism induced during sampling and the degree of the interfacial interactions (e.g., van der Waals, electrostatic, covalent) between the plasmonic substrate and analyte. Subsequent PSI treatment at high voltage conditions further impacts the overall SERS responses, where the signal sensitivity and homogeneity significantly increase throughout the entire substrate, suggesting the ready migration of adsorbed analytes regardless of their interfacial attractive forces. The PSI-induced notable SERS enhancements are presumably associated with creating unique conditions for local aggregation of the AuNPs to induce effective plasmonic couplings and hot spots (i.e., electromagnetic effect) and for repositioning analytes in close proximity to a plasmonic surface to increase polarizability (i.e., chemical effect). The optimized sampling and PSI conditions are also applicable to multi-analyte analysis by SERS and MS, with greatly enhanced detection capability and signal uniformity. Full article
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20 pages, 5404 KiB  
Article
A Sensitive SERS Sensor Combined with Intelligent Variable Selection Models for Detecting Chlorpyrifos Residue in Tea
by Hanhua Yang, Hao Qian, Yi Xu, Xiaodong Zhai and Jiaji Zhu
Foods 2024, 13(15), 2363; https://doi.org/10.3390/foods13152363 - 26 Jul 2024
Cited by 2 | Viewed by 1304
Abstract
Chlorpyrifos is one of the most widely used broad-spectrum insecticides in agriculture. Given its potential toxicity and residue in food (e.g., tea), establishing a rapid and reliable method for the determination of chlorpyrifos residue is crucial. In this study, a strategy combining surface-enhanced [...] Read more.
Chlorpyrifos is one of the most widely used broad-spectrum insecticides in agriculture. Given its potential toxicity and residue in food (e.g., tea), establishing a rapid and reliable method for the determination of chlorpyrifos residue is crucial. In this study, a strategy combining surface-enhanced Raman spectroscopy (SERS) and intelligent variable selection models for detecting chlorpyrifos residue in tea was established. First, gold nanostars were fabricated as a SERS sensor for measuring the SERS spectra. Second, the raw SERS spectra were preprocessed to facilitate the quantitative analysis. Third, a partial least squares model and four outstanding intelligent variable selection models, Monte Carlo-based uninformative variable elimination, competitive adaptive reweighted sampling, iteratively retaining informative variables, and variable iterative space shrinkage approach, were developed for detecting chlorpyrifos residue in a comparative study. The repeatability and reproducibility tests demonstrated the excellent stability of the proposed strategy. Furthermore, the sensitivity of the proposed strategy was assessed by estimating limit of detection values of the various models. Finally, two-tailed paired t-tests confirmed that the accuracy of the proposed strategy was equivalent to that of gas chromatography–mass spectrometry. Hence, the proposed method provides a promising strategy for detecting chlorpyrifos residue in tea. Full article
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12 pages, 6533 KiB  
Article
SERS Substrate Based on Ag Nanoparticles@Layered Double Hydroxide@graphene Oxide and Au@Ag Core–Shell Nanoparticles for Detection of Two Taste and Odor Compounds
by Zhixiong Lao, Mingmin Zhong, Yin Liang, Jianrong Tan, Xiaoyan Liang, Wucheng Xie, Yong Liang and Jun Wang
Chemosensors 2024, 12(7), 137; https://doi.org/10.3390/chemosensors12070137 - 11 Jul 2024
Viewed by 1283
Abstract
Sulfide organics and phenols are ubiquitous in freshwater lakes all over the world. As two taste and odor (T and O) compounds, they are harmful to the environment and human body. The existing detection methods for T and O compounds mainly include sensory [...] Read more.
Sulfide organics and phenols are ubiquitous in freshwater lakes all over the world. As two taste and odor (T and O) compounds, they are harmful to the environment and human body. The existing detection methods for T and O compounds mainly include sensory analysis and gas-phase mass spectrometry, which are cumbersome and time-consuming. Herein, a method for the simultaneous and rapid detection of two T and O compounds (methyl sulfide and 2,4-di-tert-butylphenol) based on surface-enhanced Raman spectroscopy (SERS) is firstly developed. The SERS substrate was prepared by coating Ag nanoparticles (Ag NPs), layered double hydroxide (LDH), and graphene oxide (GO) on the surface of an Ag-coated Au nanoparticle (Au@Ag NP) substrate. Under optimal conditions, this SERS substrate possessed low detection limits of 1.53 ppm for methyl sulfide and 0.39 ppm for 2,4-di-tert-butylphenol. In addition, it took only 20 min to complete the detection using this method, without complex sample pretreatment. Furthermore, it was successfully applied to simultaneously detect methyl sulfide and 2,4-di-tert-butylphenol in actual water samples and had good application prospects for the rapid detection of T and O compounds in water. Full article
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18 pages, 7377 KiB  
Article
Nanostructured Porous Silicon for Bone Tissue Engineering: Kinetics of Particle Degradation and Si-Controlled Release
by Naveen Fatima, Hamideh Salehi, Eduardo J. Cueto-Díaz, Alban Desoutter, Frédéric Cuisinier, Frédérique Cunin and Pierre-Yves Collart-Dutilleul
J. Funct. Biomater. 2023, 14(10), 493; https://doi.org/10.3390/jfb14100493 - 30 Sep 2023
Cited by 3 | Viewed by 2940
Abstract
Nanostructured porous silicon (pSi) is a synthetic silicon-based material. Its biocompatibility and bioresorbability in body fluids make pSi an appealing biomaterial for tissue engineering, with surfaces characteristics facilitating human cell adhesion and differentiation. The resorption kinetics of such porous biomaterials is crucial for [...] Read more.
Nanostructured porous silicon (pSi) is a synthetic silicon-based material. Its biocompatibility and bioresorbability in body fluids make pSi an appealing biomaterial for tissue engineering, with surfaces characteristics facilitating human cell adhesion and differentiation. The resorption kinetics of such porous biomaterials is crucial for in vivo bone regeneration, in order to adapt biomaterial resorption to tissue formation, and to control the release of loaded bioactive molecules. We investigated pSi as a bioactive scaffold for bone tissue engineering, with an emphasis on kinetics of pSi resorption and silicon release. PSi particles and chips were fabricated from crystalline silicon, and functionalized by oxidation and chemical grafting of amine groups to mimic biological structures. Materials resorption over time was investigated with Raman spectroscopy, infrared spectroscopy, and Scanning Electron Microscopy. Silicon release was followed by mass spectrometry. Particle degradation and inclusion in newly formed bone were studied in vivo. The in vitro experiments revealed that non-oxidized pSi had an accelerated initial dissolution in ddH2O and an inhibition of initial Si release in SBF. This high reactivity also led to transformation towards amorphous non-resorbable silica when incubated in SBF. PSi resorption started immediately with a maximal dissolution in the first 24 h. Later, the dissolution rate decreased over time. In comparison, the resorption process of oxidized pSi seemed delayed, but more continuous. This delayed dissolution increased the bioactivity and stability, leading to enhanced bone formation in vivo. Delayed pSi degradation provided a constant surge of silicic acid over time and promoted bone regeneration, demonstrating the high potential of pSi for bone tissue engineering: Oxidized pSi were almost completely resorbed after 2 months of healing, with remaining partially dissolved particles surrounded by newly formed bone. On the contrary, non-oxidized particles were still obviously present after 2 months with limited bone regeneration. This delayed resorption is consistent with the in vitro observations in SBF, and particles’ transformation towards silica. Full article
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16 pages, 8332 KiB  
Article
Study on Discharge Characteristics and Microstructural Evolution of PEO Coatings Based on an Al/Ti Tracer Substrate
by Guodong Li, Guang Li and Yuan Xia
Coatings 2023, 13(9), 1507; https://doi.org/10.3390/coatings13091507 - 25 Aug 2023
Cited by 2 | Viewed by 1701
Abstract
In this study, samples underwent plasma electrolytic oxidation (PEO) treatment using Al/Ti tracer substrates for 5, 10, 20, 35, and 55 min. The ionization states were determined using Optical Emission Spectroscopy (OES). Microstructural and elemental analyses were conducted using scanning electron microscopy equipped [...] Read more.
In this study, samples underwent plasma electrolytic oxidation (PEO) treatment using Al/Ti tracer substrates for 5, 10, 20, 35, and 55 min. The ionization states were determined using Optical Emission Spectroscopy (OES). Microstructural and elemental analyses were conducted using scanning electron microscopy equipped with energy dispersive spectrometry (SEM-EDS). The structural organization and phase composition of the coatings were characterized using X-ray diffraction (XRD) and Raman spectroscopy, respectively. The research findings indicate that the early discharge stage is dominated by discharge within the pre-deposited Al layer, which undergoes gradual oxidation along the thickness direction, while Ti (0.25 wt%) is found on the coating surface. The power increase was 56% of the total increase from min 5 to min 10 of discharge. As discharge time increased, the spectral peaks corresponding to Ti gradually became stronger and were accompanied by gradual enhancement of the crystallinity of the anatase and rutile phases within the coating. The coating surface displayed closed and semi-closed pores in the middle of the discharge. After 55 min of discharge, amorphous SiO2 was observed and Ti content on the coating surface increased to 4.59 wt%. Full article
(This article belongs to the Special Issue Protective Coatings in Extreme Environments)
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35 pages, 16163 KiB  
Article
Studies of Benzotriazole on and into the Copper Electrodeposited Layer by Cyclic Voltammetry, Time-of-Flight Secondary-Ion Mass Spectrometry, Atomic Force Microscopy, and Surface Enhanced Raman Spectroscopy
by Robert Mroczka and Agnieszka Słodkowska
Molecules 2023, 28(15), 5912; https://doi.org/10.3390/molecules28155912 - 6 Aug 2023
Cited by 5 | Viewed by 3988
Abstract
Benzotriazole (BTA) is an important compound that demonstrates the strongest anticorrosion properties of copper and plays a role as a leveler and an additive to the electroplating bath for control of the roughness and corrosion resistance of the electrodeposited copper layer. In this [...] Read more.
Benzotriazole (BTA) is an important compound that demonstrates the strongest anticorrosion properties of copper and plays a role as a leveler and an additive to the electroplating bath for control of the roughness and corrosion resistance of the electrodeposited copper layer. In this paper, we combined cyclic voltammetry (CV), time-of-flight secondary-ion mass spectrometry (TOF-SIMS), surface enhanced Raman spectroscopy (SERS), and atomic force microscopy (AFM) to study the interaction of BTA with copper surfaces at varied concentrations with and without the presence of chloride ions. We identified the most relevant molecular copper and its complex forms with BTA on the copper electrodeposited layer. BTA is adsorbed and incorporated into the copper surface in monomeric, dimeric, trimeric, tetrameric, and pentameric forms, inhibiting the copper electrodeposition. The addition of chloride ions diminishes the inhibiting properties of BTA. The Cu-BTA-Cl complexes were identified in the forms C12H8N6Cu2Cl and C6H4N3CuCl. Coadsorption of chloride ions and BTA molecules depends on their concentration and applied potential. Chloride ions are replaced by BTA molecules. BTA and chloride ions, depending on their concentration and applied potential, control the copper nucleation processes at the micro- and nanoscales. We compared the abilities and limitations of TOF-SIMS and SERS for studies of the interactions of benzotriazole with copper and chloride ions at the molecular level. Full article
(This article belongs to the Special Issue Recent Progress in Nanomaterials in Electrochemistry)
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