Molecularly imprinted polymers-coated magnetic covalent organic frameworks for efficient solid-phase extraction of sulfonamides in fish.

In this study, covalent organic frameworks (COFs) were grown in situ on magnetic nitrogen-doped graphene foam (MNGF), and the resulting composite of COFs-modified MNGF (MNC) was wrapped by molecularly imprinted polymers (MNC@MIPs) for specifically capturing SAs. A magnetic solid phase extraction (MSPE) method for SAs was established using MNC@MIPs with good magnetic responsiveness. The adsorption performance of MNC@MIPs was superior to that of non-molecularly imprinted polymers (MNC@NIPs), with shorter adsorption/desorption time and higher imprinting factors. A high-efficiency SAs analytical method was developed by fusing HPLC and MNC@MIPs-based MSPE. This approach provides excellent precision, a low detection limit, and wide linearity. By analyzing fish samples, the feasibility of the approach was confirmed, with SAs recoveries and relative standard deviations in spiked samples in the ranges of 77.2-112.7 % and 2.0-7.2 %, respectively. This study demonstrated the potential use of MNC@MIPs-based MSPE for efficient extraction and quantitation of trace hazards in food.

Quantum Insights into Partially Molecular Imprinted Microspheres for Anticancer Therapeutics: Experimental and Theoretical Studies.

Drug solubility is a determining factor for controlled release, and solubility-dependent release kinetics can be modified by changing the drug's state in the polymer matrix through partial molecular imprinting (PMI), although research in this area remains limited. This novel PMI approach creates nanocavities within the polymer by partially retaining the imprinting molecule and trapping the drug. Such a method holds promise for developing advanced biomaterial-based drug delivery systems for anticancer therapies. In this study, we developed microspheres designed for anticancer drug delivery utilizing PMI to enhance controlled release properties. Poly(vinyl alcohol) (PVA) microspheres were partially imprinted with aspirin (ASP) to create nanocavities for gemcitabine (GEM) molecules, inducing a polymorphic shift of GEM within the polymer matrix. This novel PMI approach enhanced drug release properties by enabling control over the drug crystallinity and release rate. The PVA-ASP-GEM complex showed zero-order release kinetics, releasing 21.6% of GEM over 48 h, maintaining steady state release profile. In contrast, nonimprinted PVA-GEM microspheres exhibited first-order kinetics with a faster release of 46.85% in the same period. Quantum insights from density functional theory (DFT) calculations revealed the superior stability of the PVA-ASP-GEM complex, with a binding free energy of -56.03 kcal/mol, compared to -29.07 kcal/mol for PVA-GEM. Molecular dynamics (MD) simulations demonstrated that ASP's presence created nanocavities that restricted GEM's movement, further contributing to the controlled release. Experimental validation through differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray diffraction (XRD), and Raman spectroscopy confirmed the polymorphic transitions within the PVA-ASP-GEM complex. This PMI-based approach offers a promising method for modulating drug release kinetics and improving the stability of anticancer therapeutics, paving the way for innovative biomaterial-based drug delivery systems.

Molecular Imprinting Technology for Advanced Delivery of Essential Oils.

Essential oils (EOs) hold therapeutic potential, but their conventional delivery systems have some limitations. This review focuses on the critical review and discussion of research related to EO delivery systems. The review also explores how molecular imprinting technologies (MIT) can advance EO delivery. MIT offer several techniques, namely covalent, non-covalent, and semi-covalent imprinting, creating targeted cavities that selectively bind and release EOs. These approaches promise significant advantages including increased selectivity, controlled release, and protection from environmental degradation. However, some challenges related to the stability and biocompatibility of MIPs remain unsolved. Integrating nanotechnology through methods like nanoparticle imprinting and some lithographic techniques seems promising to overcome these limitations. Some recently established models and systems used for EO-related research are paving the way for a more efficient and targeted EO delivery approach to harnessing the therapeutic power of EOs. Therefore, some recent and future research seems promising, and eventually it will increase the effectiveness of MIP-based EO delivery systems.

Direct detection of ethyl carbamate in baijiu by molecularly imprinted electrochemical sensors based on perovskite and graphene oxide.

Ethyl carbamate (EC), a carcinogen commonly found in Baijiu, requires an efficient detection method for quality control and monitoring. This study introduces a novel molecularly imprinted electrochemical sensor for sensitive and selective EC detection. We proposed a simple sol-gel method for the growth of perovskite-structured lanthanum manganate (LaMnO3) on graphene oxide (GO). A non-enzymatic electrochemical sensor was developed by coating a molecularly imprinted polymer synthesized via precipitation polymerization onto the surface of LaMnO3@GO. LaMnO3, with its superior three-dimensional nanocube structure, demonstrated excellent electrocatalytic activity, while the addition of GO provided a large specific surface area. The results indicate that the developed sensor exhibits exceptional recognition ability and electrochemical activity, which is attributed to the high affinity of LaMnO3@GO@MIP for EC. The sensor displays a broad linear range from 10 to 2000 µM, with a detection limit as low as 2.18 µM and long-term durability of 28 days. Notably, it demonstrates excellent selectivity, reproducibility, and stability even under different interference conditions. The sensor was successfully used to determine EC in real Baijiu samples. Overall, the sensor has broad application prospects for detecting trace contaminants in the field of food safety.

Signal amplification in molecular sensing by imprinted polymers.

In the field of sensing, the development of sensors with high sensitivity, accuracy, selectivity, sustainability, simplicity, and low cost remains a key focus. Over the past decades, optical and electrochemical sensors based on molecular imprinting techniques have garnered significant attention due to the above advantages. Molecular imprinting technology utilizes molecularly imprinted polymers (MIPs) to mimic the specific recognition capabilities of enzymes or antibodies for target molecules. Recently, MIP-based sensors rooting in signal amplification techniques have been employed to enhance molecular detection level and the quantitative ability for environmental pollutants, biomolecules, therapeutic compounds, bacteria, and viruses. The signal amplification techniques involved in MIP-based sensors mainly cover nucleic acid chain amplification, enzyme-catalyzed cascade, introduction of high-performance nanomaterials, and rapid chemical reactions. The amplified analytical signals are centered around electrochemical, fluorescence, colorimetric, and surface-enhanced Raman techniques, which can effectively realize the determination of some low-abundance targets in biological samples. This review highlights the recent advancements of electrochemical/optical sensors based on molecular imprinting integrated with various signal amplification strategies and their dedication to the study of trace biomolecules. Finally, future research directions on developing multidimensional output signals of MIP-based sensors and introducing multiple signal amplification strategies are proposed.

Sensitive Coatings Based on Molecular-Imprinted Polymers for Triazine Pesticides' Detection.

Triazine pesticide (atrazine and its derivatives) detection sensors have been developed to thoroughly check for the presence of these chemicals and ultimately prevent their exposure to humans. Sensitive coatings were designed by utilizing molecular imprinting technology, which aims to create artificial receptors for the detection of chlorotriazine pesticides with gravimetric transducers. Initially, imprinted polymers were developed, using acrylate and methacrylate monomers containing hydrophilic and hydrophobic side chains, specifically for atrazine, which shares a basic heterocyclic triazine structure with its structural analogs. By adjusting the ratio of the acid to the cross-linker and introducing acrylate ester as a copolymer, optimal non-covalent interactions were achieved with the hydrophobic core of triazine molecules and their amino groups. A maximum sensor response of 546 Hz (frequency shift/layer height equal to 87.36) was observed for a sensitive coating composed of 46% methacrylic acid and 54% ethylene glycol dimethacrylate, with a demonstrated layer height of 250 nm (6.25 kHz). The molecularly imprinted copolymer demonstrated fully reversible sensor responses, not only for atrazine but also for its metabolites, like des-ethyl atrazine, and structural analogs, such as propazine and terbuthylazine. The efficiency of modified molecularly imprinted polymers for targeted analytes was tested by combining them with a universally applicable quartz crystal microbalance transducer. The stable selectivity pattern of the developed sensor provides an excellent basis for a pattern recognition procedure.

Highly selective ethanol vapour sensing materials for a new generation of gas sensors based on molecularly imprinted polymers.

A simple gas sensor consisting of a molecularly imprinted polymer-carbon nanotube composite cast onto a screen-printed electrode has been developed with extremely high selectivity for ethanol vapour over methanol vapour. Ethanol gas sensors typically display selectivity for ethanol over methanol in the range 2-4 times, while the mean ratio of ethanol to methanol response observed with the described device was 672. This selectivity was achieved under ambient conditions. Additionally, the molecularly imprinted polymer was produced using reagents previously applied in the development of a device selective for methanol, with only the template being changed. This demonstrates the versatility of molecular imprinting and provides a foundation for their greater integration into future gas sensors.

Metabolic landscaping of extracellular vesicles from body fluids by phosphatidylserine imprinted polymer enrichment and mass spectrometry analysis.

Extracellular vesicles (EVs) are emerging as new source of biomarkers discovery in liquid biopsy due to their stabilization in body fluids, protected by phospholipid bilayers. However, the metabolomics study of EVs is very little reported due to the lack of efficient and high-throughput isolation methods for clinical samples. In this study, phosphatidylserine imprinted polymers were employed for rapid and efficient EVs isolation from five human body fluids, including plasma, urine, amniotic fluid, cerebrospinal fluid, and saliva. The isolated EVs were subsequently analyzed for metabolomic studies by high-resolution mass spectrometry. Metabolic landscaping was conducted between the body fluids and their EVs, indicating EVs contain a large number of metabolites that are completely specific to the body fluid source. Finally, quantitative metabolomic analysis of EVs was carried out with plasma samples of hepatocellular carcinoma. Several differentially expressed exosomal metabolites were revealed including the upregulation of sphingosine (d18:1), taurochenodeoxycholic acid (TCDCA), pipecolic acid (PA), and 4-hydroxynonenal (4-HNE) and down-regulation of piperine, caffeine, and indole. We believe the proposed methodology will provide a deeper understanding of the molecular composition and functions of EVs as an alternative source for biomarker discovery.

Polyvinylidene Fluoride-Based Nanowire-Imprinted Membranes with High Flux for Efficient and Selective Separation of Artemisinin/Artemether.

A traditional phase transformation method is commonly used to prepare molecular imprinting membranes for selective separation. However, traditional molecularly imprinted polymers are mostly micron-sized particles, and the imprinting sites in their membrane are easily embedded, leading to a reduced adsorption capacity and decreased selectivity. In this study, an ultra-long nanowire with a diameter of about 15 nm was synthesized for the separation of artemisinin (ART), and its adsorption capacity was as high as 198.29 mg g-1 after imprinting polymerization. Molecular imprinting membranes were prepared, using polyvinylidene fluoride (PVDF), polyethersulfone (PES), and polysulfone (PSF) as the membrane matrix, for comparison. The average membrane pore size of PVDF-MIM was about 480 nm, and PVDF-MIM had the highest adsorption capacity (69 mg g-1) for ART. The optimal flow rate for PVDF-MIM's dynamic adsorption of ART was 7 mL min-1. Under this optimal flow rate, selectivity experiments were carried out to obtain the separation factor of PVDF-MIM (α = 8.37), which was much higher than the corresponding values of PES-MIM and PSF-MIM. In addition, the hydrophobicity and low flux of PES-MIM and PSF-MIM lead to higher non-specific adsorption. The hydrophobicity of PVDF-MIM is lower than that of PES-MIM and PSF-MIM, which greatly reduces the non-specific adsorption of the membrane, thus increasing the selectivity of the membranes. Therefore, the effective density of the imprinting sites in the pores and the membrane structure are the main factors determining the efficient separation of molecularly imprinted membranes.

Rational Design of Non-Covalent Imprinted Polymers Based on the Combination of Molecular Dynamics Simulation and Quantum Mechanics Calculations.

Molecular imprinting is a promising approach for developing polymeric materials as artificial receptors. However, only a few types of molecularly imprinted polymers (MIPs) are commercially available, and most research on MIPS is still in the experimental phase. The significant limitation has been a challenge for screening imprinting systems, particularly for weak functional target molecules. Herein, a combined method of quantum mechanics (QM) computations and molecular dynamics (MD) simulations was employed to screen an appropriate 2,4-dichlorophenoxyacetic acid (2,4-D) imprinting system. QM calculations were performed using the Gaussian 09 software. MD simulations were conducted using the Gromacs2018.8 software suite. The QM computation results were consistent with those of the MD simulations. In the MD simulations, a realistic model of the 'actual' pre-polymerisation mixture was obtained by introducing numerous components in the simulations to thoroughly investigate all non-covalent interactions during imprinting. This study systematically examined MIP systems using computer simulations and established a theoretical prediction model for the affinity and selectivity of MIPs. The combined method of QM computations and MD simulations provides a robust foundation for the rational design of MIPs.

Molecular imprinting electrochemical sensor based on hollow spherical PProDOT-2CH2OH and chitosan-derived carbon materials for highly sensitive detection of chloramphenicol.

The misuse of chloramphenicol (CAP) has jeopardized environmental safety. It is critical to create an effective and sensitive CAP detection technique. In this paper, a composite of chitosan (CS)-derived carbon material modified hollow spherical hydroxylated poly(3,4-propylenedioxythiophene) (PProDOT-2CH2OH) was designed, which innovatively used o-phenylenediamine and p-aminobenzoic acid as bi-functional monomers to prepare molecular imprinting polymer (MIP) sensors for highly sensitive analysis and determination of CAP. It was found that the hollow spherical structure of PProDOT-2CH2OH significantly enhanced the rapid electron migration. When combined with the CS-derived carbon material, which has multi-functional sites, it improved the electrical activity and stability of the sensor. It also provided more active centers for the MIP layer to specifically recognize CAP. Therefore, this MIP sensor had a wide linear response (0.0001 ∼ 125 µM), a low limit of detection (LOD, 6.6 pM), excellent selectivity and stability. In addition, studies showed that the sensor has potential practical value. ENVIRONMENTAL IMPLICATION: Chloramphenicol (CAP) is one of the most widely used antibiotics with the highest dosage due to its low price and broad-spectrum antimicrobial properties. Due to its incomplete metabolism in living organisms and its difficulty in degrading in the environment, contamination caused by it can pose a threat to public health. In this study, a novel molecularly imprinted sensor (MIP/PC2C1/GCE) was designed to provide a new idea for rapid and precise removal of CAP by adsorption. The detection of CAP in pharmaceutical, water quality, and food fields was realized.

A molecular imprinted ratiometric fluorescence sensor based on blue/orange MXene quantum dots for visual detection of histamine.

Histamine is a highly toxic biogenic amine in food, making its sensitive and rapid detection methods vital for the assurance of edible safety and human health. Here, we explored for the first time a smartphone-enabled ratiometric imprinted fluorescence sensor based on blue/orange MXene quantum dots (MQDs) for fluorescence and visual detection of histamine. A linear relationship between the concentration of histamine and the fluorescence response of the sensor was found in the range of 1-60 µM with a limit of detection (LOD) of 21.9 nM for fluorescence detection and 92.2 nM for visual detection. In addition, the method was validated for the detection of real samples with excellent recoveries from 96.52% to 105.32%. Therefore, this work greatly expands the application of MQDs in the fluorescence sensing field, as well as provides a visual strategy for in-situ detection of histamine in food.

Molecularly imprinted Photoelectrochemical sensor for Escherichia coli based on Cu:ZIF-8/KZ3TTz heterojunction.

Herein, a signal stable molecularly imprinted photoelectrochemical (MIP-PEC) sensing platform was designed to sensitively detect Escherichia coli by incorporating polythiophene film with Cu: ZIF-8/KZ3TTz heterojunction. Attributed to the formation of a staggered type II heterostructure between KZ3TTz and Cu: ZIF-8 semiconductors, the Cu: ZIF-8/KZ3TTz heterojunction exhibited stable and significant cathode PEC response. Impressively, selective MIP film was grown on the surface of Cu: ZIF-8/KZ3TTz/GCE by electro-polymerization of 2,2-Dimethyl-5-(3-thienyl)-1,3-dioxane-4,6-dione (DTDD) in the presence of E. coli. After removing E. coli, more electrons were transferred to the electrolyte solution through the imprinting cavity on the MIP film, which was eliminated by O2 in the electrolyte, causing further enhancement of the cathode PEC response. On the contrary, when the imprinted cavity was filled with E. coli, the cathodic PEC response gradually decreased due to steric hindrance effect. The sensor showed excellent linearity in the range of 101 to 108 CFU/mL with a detection limit of 4.09 CFU/mL (S/N = 3). This strategy offered a novel approach for pathogenic bacteria detection in food safety and environmental monitoring.

Antimicrobial assay and controlled drug release studies with novel eugenol imprinted p(HEMA)-bacterial cellulose nanocomposite, designed for biomedical applications.

In this study, a novel bio-composite material that allow sustained release of plant derived antimicrobial compound was developed for the biomedical applications to prevent the infections caused by microorganisms resistant to commercial antimicrobials agents. With this aim, bacterial cellulose (BC)-p(HEMA) nanocomposite film that imprinted with eugenol (EU) via metal chelated monomer, MAH was prepared. Firstly, characterization studies were utilized by FTIR, SEM and BET analysis. Then antimicrobial assays, drug release studies and in vitro cytotoxicity test were performed. A significant antimicrobial effect against both Gram (+) Staphylococcus aureus and Gram (-) Escherichia coli bacteria and a yeast Candida albicans were observed even in low exposure time periods. When antimicrobial effect of EU compared with commercially used agents, both antifungal and antibacterial activity of EU were found to be higher. Then, sustained drug release studies showed that approximately 55% of EU was released up to 50 h. This result proved the achievement of the molecular imprinting for an immobilization of molecules that desired to release on an area in a long-time interval. Finally, the in vitro cytotoxicity experiment performed with the mouse L929 cell line determined that the synthesized EU-imprinted BC nanocomposite was biocompatible.

Two-Dimensional Estrone-Imprinted System on a Self-Assembled Monolayer.

In this study, a thin poly (methyl methacrylate) coating was formed on a self-assembled monolayer formed on a gold plate after chemically binding estrone. Subsequently, the estrone molecules were hydrolyzed and extracted using a solvent to form a molecular-imprinted system. The estrone-imprinted gold plate was then used as a working electrode to measure the estrone recognition ability through electrochemical methods. The recognition ability of this working electrode was evaluated for similar compounds. The selectivity factors for the seven estrone analogs were measured, and these values ranged from 0.19 to 0.67. According to the experimental results, the estrone-imprinted system showed good differentiation of estrone from other estrone analogs. Comparing these selectivity factors with those of a previous study on a cholesterol-imprinted system, the relative molecular size difference between the target molecule and similar molecules had a significant impact on the selectivity factor.

Thiram Determination in Milk Samples by Surface Plasmon Resonance Based on Molecularly Imprinted Polymers and Sulphur-Doped Titanium Dioxide.

In this work, a new surface plasmon resonance (SPR) sensor based on sulphur-doped titanium dioxide (S-TiO2) nanostructures and molecularly imprinted polymer (MIP) was presented for thiram (THI) determination in milk samples. Firstly, the S-TiO2 nanomaterial with a high product yield was prepared by using a facile sol-gel hydrolysis technique with a high product yield. After that, UV polymerization was carried out for the preparation of the THI-imprinted SPR chip based on S-TiO2 using a mixture including ethylene glycol dimethacrylate (EGDMA) as the cross-linker, N,N'-azobisisobutyronitrile (AIBN) as the initiator, and methacryloylamidoglutamicacid (MAGA) as the monomer. The reliability of the sensor preparation procedure has been successfully proven by characterization studies of the prepared nanomaterials and SPR chip surfaces through spectroscopic, microscopic, and electrochemical methods. As a result, the prepared SPR sensor showed linearity in the range of 1.0 × 10-9-1.0 × 10-7 M with a detection limit (LOD) of 3.3 × 10-10 M in the real samples, and a sensor technique for THI determination with high sensitivity, repeatability, and selectivity can be included in the literature.

Dual Template Molecularly Imprinted Polymers Targeting Blockade of CD47 for Enhanced Macrophage Phagocytosis and Synergistic Antimetabolic Therapy.

Glycinamide ribonucleotide formyltransferase (GARFT) is an important enzyme in the folate metabolism pathway, and chemical drugs targeting GARFT have been used in tumor treatments over the past few decades. The development of novel antimetabolism drugs that target GARFT with improved performance and superior activity remains an attractive strategy. Herein, we proposed a targeted double-template molecularly imprinted polymer (MIP) for enhancing macrophage phagocytosis and synergistic antimetabolic therapy. The double-template MIP was prepared by imprinting the exposed peptide segment of the extracellular domain of CD47 and the active center of GARFT. Owing to the imprinted cavities on the surface of MIP, it can actively target cancer cells and mask the "do not eat me" signal upon binding to CD47 thereby blocking the CD47-SIRPα pathway and ultimately enhancing phagocytosis by macrophages. In addition, MIP can specifically bind to the active center of GARFT upon entry into the cells, thereby inhibiting its catalytic activity and ultimately interfering with the normal expression of DNA. A series of cell experiments demonstrated that MIP can effectively target CD47 overexpressed 4T1 cancer cells and inhibit the growth of 4T1 cells. The enhanced phagocytosis ability of macrophages-RAW264.7 cells was also clearly observed by confocal imaging experiments. In vivo experiments also showed that the MIP exhibited a satisfactory tumor inhibition effect. Therefore, this study provides a new idea for the application of molecular imprinting technology to antimetabolic therapy in conjunction with macrophage-mediated immunotherapy.

A molecularly imprinting photoelectrochemical sensor based on Bi2O2S-sensitized perovskite Cs2AgBiBr6 for sarcosine determination.

An original molecular imprinting photoelectrochemical (PEC) sensor for sarcosine detection based on stable lead-free inorganic halide double perovskite Cs2AgBiBr6 is proposed. Cs2AgBiBr6 as a lead-free halide perovskite material possesses several positive optoelectronic properties for PEC analysis, such as long-lived component to the charge-carrier lifetime, and strong absorption of visible light. At the same time, two-dimensional materials also offer excellent electronic and mechanical properties; thus, Bi2O2S was used and combined with Cs2AgBiBr6 to provide a stable and large photocurrent, which also benefits from the  stability of perovskite Cs2AgBiBr6. Based on this novel PEC assay, the detection range for sarcosine was between 0.005 and 5000 ng/mL with a low detection limit of 0.002 ng/mL. This work also improved the adhibition of metal halide perovskite in analytical chemistry field, providing a novel way for other small molecule detection.

Co2+ coordination-assisted molecularly imprinted covalent organic framework for selective extraction of ochratoxin A.

Covalent organic frameworks (COFs) are attractive materials for sample pretreatment due to their tunable structures and functions. However, the precise recognition of contaminant in complex environmental matrices by COFs remains challenging owing to their insufficient specific active sites. Herein, we report Co2+ coordination-assisted molecularly imprinted flexible COF (MI-COF@Co2+) for selective recognition of ochratoxin A (OTA). The MI-COF@Co2+ was prepared via one-step polymerization of 3,3-dihydroxybenzidine, 2,4,6-tris(4-formylphenoxy)- 1,3,5-triazine, Co2+ and template. The flexible units endowed COFs with the self-adaptable ability to regulate the molecular conformation and coordinate with Co2+ to locate the imprinted cavities. The coordination interaction greatly improved the adsorption capacity and selectivity of MI-COF@Co2+ for OTA. The prepared MI-COF@Co2+ was used as solid phase extraction adsorbent for high-performance liquid chromatography determination of OTA with the detection limit of 0.03 ng mL-1 and the relative standard deviation of < 2.5 %. In addition, this method permitted interference-free determination of OTA in real samples with recovery from 89.5 % to 102.8 %. This work provides a simple way to improve the selectivity of COFs for the determination of hazardous compounds in complex environments.

Nanofibrous Conductive Sensor for Limonene: One-Step Synthesis via Electrospinning and Molecular Imprinting.

Detecting volatile organic compounds (VOCs) emitted from different plant species and their organs can provide valuable information about plant health and environmental factors that affect them. For example, limonene emission can be a biomarker to monitor plant health and detect stress. Traditional methods for VOC detection encounter challenges, prompting the proposal of novel approaches. In this study, we proposed integrating electrospinning, molecular imprinting, and conductive nanofibers to fabricate limonene sensors. In detail, polyvinylpyrrolidone (PVP) and polyacrylic acid (PAA) served here as fiber and cavity formers, respectively, with multiwalled carbon nanotubes (MWCNT) enhancing conductivity. We developed one-step monolithic molecularly imprinted fibers, where S(-)-limonene was the target molecule, using an electrospinning technique. The functional cavities were fixed using the UV curing method, followed by a target molecule washing. This procedure enabled the creation of recognition sites for limonene within the nanofiber matrix, enhancing sensor performance and streamlining manufacturing. Humidity was crucial for sensor working, with optimal conditions at about 50% RH. The sensors rapidly responded to S(-)-limonene, reaching a plateau within 200 s. Enhancing fiber density improved sensor performance, resulting in a lower limit of detection (LOD) of 137 ppb. However, excessive fiber density decreased accessibility to active sites, thus reducing sensitivity. Remarkably, the thinnest mat on the fibrous sensors created provided the highest selectivity to limonene (Selectivity Index: 72%) compared with other VOCs, such as EtOH (used as a solvent in nanofiber development), aromatic compounds (toluene), and two other monoterpenes (α-pinene and linalool) with similar structures. These findings underscored the potential of the proposed integrated approach for selective VOC detection in applications such as precision agriculture and environmental monitoring.