Microchimica Acta最新文献_第5页

Simultaneous enrichment and ultra-high sensitivity detection of multi-structural synthetic cannabinoids in large-volume wastewater

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-04-07 DOI: 10.1007/s00604-025-07128-7

Rui Cao, Jiawei Chen, Ningjia Pang, Siyu Li, Mengyi Chen, Bin Di, Deli Xiao

Nowadays, the abuse of synthetic cannabinoids has aroused the world’s great attention. However, the determination of synthetic cannabinoids in wastewater faces the bottleneck of complex species and very low content. Therefore, this work integrated GO-Fe₃O₄ with an ionic liquid (ILs-GO-Fe₃O₄) to create a mixed hemimicelles magnetic solid-phase extraction (MHMSPE) system for the detection of synthetic cannabinoids (SCs) in wastewater samples using ultrahigh-performance liquid chromatography—tandem mass spectrometry (UHPLC-MS/MS). Because of the multiple interaction sites of mixed hemimicelles’ magnetic solid-phase extraction materials, multi-structural synthetic cannabinoids can be enriched simultaneously. Under the optimized conditions, the limits of quantitation (LOQ) of the method were as low as 10–50 pg/L, lower than other methods. The average recoveries of 18 analytes were in the range 71.23–96.08% with relative standard deviations (RSD) lower than 15% (n = 6). To our knowledge, this is the first development of magnetic solid-phase extraction for large-volume samples pretreatment (1 L) and ultra-high sensitive detection of synthetic cannabinoids (10 pg/L), due to the high enrichment factor (10,000-fold). The extraction process was convenient, accurate, and rapid, and offers significant potential for ultra-high sensitivity detection in large-volume samples, providing a valuable tool for simultaneous broad-spectrum extraction and drug abuse monitoring.

Graphical abstract

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引用次数: 0

Light-driven in situ deposited Au nanoparticles on ZnO substrate with ultrasensitive SERS enhancement for molecular detection

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-04-06 DOI: 10.1007/s00604-025-07118-9

Apichaya Chantaraklud, Chanoknan Rattanabut, Suwussa Bamrungsap, Tanujjal Bora

Uniform, reproducible and stable SERS substrates with high detection sensitivity are crucial for their successful commercial applications. Here, we introduce a plasmonic SERS substrate based on gold nanoparticles (AuNPs) fabricated by using a straightforward light-driven in-situ method for highly sensitive molecular detection. A dense array of zinc oxide nanorods (ZnO NRs) was used as a support surface for the in-situ growth of Au nanoparticles (AuNPs). The SERS performance of the fabricated Au-ZnO substrates was evaluated by using rhodamine 6G (R6G) dye as a model Raman probe, where the distribution of the AuNPs on the substrate was found to play an important role defining the SERS activities The Au-ZnO substrates exhibited exceptional homogeneity (RSD = 3.95%), a detection limit (LOD) of 9 × 10^–11 M, and signal enhancement in the order of 10⁶. Additionally, these substrates demonstrated good stability over a period of 4 weeks when stored under standard room conditions, maintaining more than 80% of the initial Raman signal intensity. When tested for antibiotic residue detection in water using amoxicillin as a model antibiotic, the Au-ZnO substrates revealed LOD in the order of 10^–9 M with linear detection over a wide concentration range of amoxicillin in water. The present work offers a straightforward and inexpensive solution-processed fabrication approach for SERS substrates that holds great potential for the development of extremely sensitive and reliable SERS-based detection and sensor systems.

Graphical abstract

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引用次数: 0

Nanomaterials functionalized signal-ON/OFF electrogenerated chemiluminescence biosensor for quantization of trypsin based on target-induced cleavage of peptide

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-04-04 DOI: 10.1007/s00604-025-07131-y

Shuo Kang, Ronghan Qu, Yuhong Duan, Jiale Yang, Fen Ma

Trypsin (TPN) is an important proteolytic enzyme in the digestive system and its abnormal levels are indicative of some pancreatic diseases. As an endopeptidase, TPN can cleave substrate peptide mainly by catalyzing the hydrolysis of the carboxyl side peptide bond of lysine (K) or arginine (R) residues. Based on this hydrolysis cleavage effect, two kinds of nanomaterials functionalized electrogenerated chemiluminescence (ECL) biosensors for the determination of TPN were designed as follows: A signal-ON ECL biosensor was fabricated by attaching substrate peptide (HWR*GWVC, “*” representing the cleavage site, abbreviated as HGC) labeled with ferrocene carboxylic acid (as quencher) onto the surface of NH₂-MIL-53(Al) film which was incorporated with ECL emitting species (bis (2,2′-bipyridine)-4′-methyl-4-carboxybipyridine-ruthenium (N-succinimidylester)-bis (hexafluorophosphate) (Ru complex)). The presence of tryptic cleavage event can eventually lead the Fc complex to leave the electrode and results in the increase of the ECL intensity. HGC labeled with Ru-Ti₃C₂T_x-AuNP complex was used as capture probe and signal probe, which was attached onto NH₂-MIL-53(Al) film modified glassy carbon electrode. A signal-OFF ECL biosensor was built as described above. The presence of TPN lead the Ru-Ti₃C₂T_x-AuNPs to leave the electrode, which resulted in the decreasing ECL intensity. As expected, the fabricated ECL biosensing methods provide excellent sensitivity and selectivity toward the TPN activity. Thus, this strategy shows great potential application in the clinic for diagnosis of TPN-indicating diseases as well as the screening of TPN inhibitor-based anti-cancer drugs.

Graphical abstract

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引用次数: 0

A highly selective electrochemical aptasensor for Pb2+ based on molecular imprinting technology and tetrahedral DNA nanostructure

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-04-02 DOI: 10.1007/s00604-025-07101-4

Jiaqi Han, Nianxin Zhu, Jiahao Sha, Jinyan Cai, Hui Cao, Tai Ye, Liling Hao, Fei Xu

A novel electrochemical biosensor for the detection of lead ions (Pb²⁺) with improved specificity and sensitivity was developed. The sensor design incorporated molecular imprinting technology, where chitosan was polymerized on the electrode surface to form a lead-specific cavity structure, thereby enhancing selectivity in complex sample matrices. Meanwhile, the tetrahedral DNA nanostructure was employed as the recognition probe to mitigate the entanglement issues commonly associated with single-stranded DNA, thus improving the sensitivity of the detection. The developed sensor exhibited a linear dynamic range from 0.050 to 2.000 μg/mL, with a limit of detection (LOD) of 0.0034 μg/mL. The aptasensor’s efficacy was verified through the analysis of aquatic samples, demonstrating a high degree of reliability comparable to that of inductively coupled plasma mass spectrometry (ICP-MS).

Graphical Abstract

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引用次数: 0

Silica-based optical chemosensors for rapid and reliable on-site detection of gamma-hydroxybutyrate in beverages and oral fluids

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-04-02 DOI: 10.1007/s00604-025-07134-9

Jordi Hernández-Contreras, Jordi Roig-Rubio, Margarita Parra, Salvador Gil, Pau Arroyo, José A. Sáez, Carlos Lodeiro, Pablo Gaviña

The illicit use of gamma-hydroxybutyrate (GHB) in drug-facilitated crimes underscores the urgent need for rapid and reliable detection technologies. This study introduces two innovative silica-based nanosensors that offer real-time, on-site detection of GHB in spiked beverages at concentrations typical of chemical submission cases. Both chemosensors are based on silica nanoparticles functionalized with 2-aminonaphtoxazole derivatives. The first nanosensor, modified with a p-nitroaniline chromogenic unit, enables a visible color change for immediate visual identification, while the second incorporates a fluorescein derivative for high-sensitivity detection via fluorescence. Both nanosystems demonstrate exceptional specificity to GHB, with minimal interference from other substances. Moreover, the solid-phase integration of these nanosensors onto hydrophobic cellulose-based substrates enhances their portability and user-friendliness, making them suitable for nightlife venues and forensic applications. Finally, chromogenic precursor 1 has proven to be an excellent chemosensor for the visual detection of GHB in oral fluid, with a calculated LOD of 19.2 μM, and a linear response in the 32–132 μM range.

Graphical abstract

γ-羟丁酸（GHB）在毒品犯罪中的非法使用凸显了对快速可靠检测技术的迫切需求。本研究介绍了两种基于二氧化硅的创新型纳米传感器，可现场实时检测加标饮料中的 GHB，检测浓度通常为化学品呈递案件中的典型浓度。这两种化学传感器都基于用 2-aminonaphtoxazole 衍生物功能化的二氧化硅纳米粒子。第一种纳米传感器由对硝基苯胺发色单元修饰，能产生可见的颜色变化，可立即进行视觉识别；第二种纳米传感器则加入了荧光素衍生物，可通过荧光进行高灵敏度检测。这两种纳米系统对伽马--羟丁酸（GHB）都具有极高的特异性，受其他物质的干扰极小。此外，将这些纳米传感器固相集成到疏水性纤维素基底上还增强了它们的便携性和易用性，使其适用于夜生活场所和法医应用。最后，色原前体 1 被证明是目视检测口腔液中伽马--羟丁酸（GHB）的极佳化学传感器，其计算 LOD 为 19.2 μM，在 32-132 μM 范围内呈线性响应。

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引用次数: 0

Cauliflower-like CuO-ZnO modified glassy carbon electrode as an electrochemical platform for the detection of hydrogen peroxide in adulterated milk

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-04-01 DOI: 10.1007/s00604-025-07130-z

Haiyan Song, Haobin Hu, Zhijun Li, Yun Wu, Chunxiao He, Yuanyuan Gao, Nana Hou, Qiqi He, Zhenyu Cheng

The detection of hydrogen peroxide (H₂O₂) is a crucial process in various industries, including food safety. In this study, a cauliflower-like CuO-ZnO composite with p–n junction was successfully synthesized using a straightforward one-pot hydrothermal method. The resulting material demonstrates outstanding electrocatalytic performance for H₂O₂ detection, outperforming the individual components. The electrochemical sensor constructed from the cauliflower-like CuO-ZnO composite exhibits a well-defined linear response in the concentration range 0.0005 to 0.105 mmol·L⁻¹ for H₂O₂. The sensor’s limit of detection (LOD) is 0.21 µmol·L⁻¹ at a signal-to-noise ratio (S/N) of 3, with a sensitivity of 1582.7 µA·(mmol·L⁻¹)⁻¹·cm⁻². Furthermore, the sensor has been successfully applied to detect trace amounts of H₂O₂ in milk samples, showcasing its potential for sensitive electrochemical sensing applications.

Graphical Abstract

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引用次数: 0

Assembly of adaptive engineering aptamers for Escherichia coli and their application in all-in-one rapid detection

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-04-01 DOI: 10.1007/s00604-025-07138-5

Mengyue Liu, Shicai Xu, Giovanna Marrazza

Multivalent engineering aptamers (multi-Apts) adaptive and specific to whole Escherichia coli (E. coli: CMCC 44102) cells based on hybridization chain reaction (HCR) were constructed for the first time. The dissociation constant (K_d) value for these multi-Apts was 48 nM, demonstrating a higher affinity than that of monovalent aptamers (mono-Apts) (K_d = 102 nM). Furthermore, the reaction equilibrium of multi-Apts was achieved within 20 min, with a reaction rate twice that of mono-Apts. To validate the exceptional performance of these multi-Apts, they were employed as recognition elements in conjunction with gold nanoparticles (AuNPs) colorimetric assays for the all-in-one rapid detection of E. coli. This method exhibited a linear detection range from 1 × 10² to 1 × 10⁷ CFU mL⁻¹, achieving a limit of detection (LOD) as low as 19 CFU mL⁻¹. The recovery of this method in tap water and milk were 85.7% to 101% and 81.8% to 98.2%, respectively. The results indicated that this method not only provided a wide detection range but also exhibited high sensitivity and accuracy. Additionally, this study demonstrated that multi-Apts possessed greater application potential in the detection of macromolecular substances such as bacteria. In short, this work provided a novel approach for rapid and all-in-one detection of E. coli in food.

Graphical Abstract

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引用次数: 0

Design and application of graphene oxide-based molecularly imprinted covalent organic framework for simultaneous and precise recognition of bile acid metabolites

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-03-31 DOI: 10.1007/s00604-025-07120-1

Yue Yuan, Tianyi Xue, Mengxin Ren, Yanzhu Liu, Zhexue Song, Zhili Xiong, Feng Qin

In this study a bile acid (BA)-imprinted covalent organic framework (COF) was constructed via Schiff base reactions, which integrated the advantages of both inherent structural stability of COF and exceptional selectivity of molecular imprinting technology. Besides, it was found that the addition of graphene oxide (GO) effectively increased the dispersibility of nanoparticles, ultimately resulting in a GO-based molecularly imprinted COF (GO@MICOF). The GO@MICOF was identified with the characteristics of excellent mass transfer performance (20.09 mg g^–1), specific surface area (152.35 m² g^–1), selectivity (IFs = 2.4), and regeneration ability (n ≥ 10). By coupling the GO@MICOF-based pretreatment method with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis, sensitive and accurate validation results (LOQs, 0.01–2.5 µmol L^–1; extraction efficiency, 81.1–118.9%) were obtained. Notably, the application of the proposed pretreatment techniques to metabolomics analysis holds great significance for the precision of metabolomics results. Sixteen BA metabolites were successfully quantified in rat liver and fecal samples, and some potential biomarkers and related metabolic pathways associated with postmenopausal osteoporosis had been identified. Therefore, the integrated analysis strategy has significant advantages in purifying complex biological samples and has great application prospects in targeted metabolomics research.

Graphical abstract

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引用次数: 0

Handling electric connections in 3D-printed electrodes and sensors

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-03-28 DOI: 10.1007/s00604-025-07122-z

Ivan Verlangieri, Thawan Gomes de Oliveira, Fernando Silva Lopes, Ivano Gebhardt Rolf Gutz, Lúcio Angnes, Claudimir Lucio do Lago

Voltammetric and amperometric sensors typically consist of an electroactive surface, an electrode substrate, and connection tracks. While metal connectors exhibit negligible resistance, semiconductor materials, conductive polymers, or composites can introduce significant electrical resistance. This study investigates the electrical behavior of 3D-printed conductive polymer tracks and metal connections, focusing on limitations and improvements. Carbon black PLA (CB-PLA) was chosen for its favorable electrical properties. Printed tracks showed higher resistivity (17 Ω·cm) than the raw filament (6 Ω·cm). The electrical contact resistance (ECR) between nickel-plated metals and CB-PLA ranged from 10² to 10³ Ω. Pressed contacts (e.g., alligator clips) were unstable and introduced noise, while a welded metal-polymer contact (WMPC), achieved via induction heating, improved stability. Despite high resistivity, the electrochemical behavior remained unaffected, apart from an Ohmic drop requiring compensation for accurate sensor performance. To address this, a four-electrode potentiostat was proposed for dynamic Ohmic drop compensation. Cyclic voltammetry experiments were performed using a custom 3D-printed electrode with dual conducting tracks to independently monitor potential and current. Results from a commercial four-electrode potentiostat were compared with those from a conventional three-electrode system. A four-electrode potentiostatic module (FEPM) was developed for compatibility with standard three-electrode instruments, yielding comparable results. Peak current varied linearly with hexaammineruthenium(III) concentration (R² = 0.992) and with the square root of the scan rate (R² ≥ 0.993). Differential pulse voltammetry confirmed enhanced performance with the four-electrode setup. These findings highlight key considerations for integrating 3D-printed components into electrochemical systems and mitigating ECR and Ohmic drop.

Graphical Abstract

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引用次数: 0

Laccase-mimicking enzyme with fluorescent properties for dual-mode detection of epinephrine and degradation of phenolic pollutants

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta

Pub Date : 2025-03-28 DOI: 10.1007/s00604-025-07069-1

Huizhu Fan, Luxi Huang, Yin Dai, Hongsong Zhang, Wanying Zhu, Jun Zhang, Junli Hong

Despite considerable interest has been shown in research on nanozymes in recent times, the creation of highly active bifunctional nanozymes remains a significant challenge. Inspired by the structural features of the active center of natural laccase, bifunctional copper-based nanozymes (Cu-MB) possessing both laccase-like activity and fluorescence properties using 2-methylimidazole (2-MI) and 2-aminoterephthalic acid (BDC-NH₂) as ligands have been prepared. The K_m of Cu-MB was 0.0898 mM, which was markedly lower than that of previously reported nanozymes and natural laccase. A dual-mode sensor for the detection of epinephrine (EP) was designed based on the high catalytic activity, excellent fluorescence properties, and stability of Cu-MB nanozymes. The limits of detection (LODs) of the colorimetric and fluorescence sensors for EP were 0.22 µg/mL and 0.11 µg/mL, respectively. The sensor system was verified to have good resistance to interferences and reliability by analyzing actual samples. Furthermore, the integration of a dual-reading hydrogel with a smartphone facilitates the portable, real-time, and rapid assessment of EP. More encouragingly, Cu-MB has excellent substrate versatility and can effectively degrade a diverse array of phenolic pollutants. The developed Cu-MB nanozymes provide a promising approach for the degradation and determination of phenolic compounds. Clinical trial number: not applicable.

Graphical abstract

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引用次数: 0