Analytica Chimica Acta最新文献

英文中文

Size assessing of different silica-based materials by asymmetrical flow field flow fractionation: from nanometers to micrometers 通过不对称流场流动分选对不同硅基材料的尺寸进行评估：从纳米到微米

IF 6 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-15 Epub Date: 2026-01-29 DOI: 10.1016/j.aca.2026.345162

L. Sanjuan-Navarro, P. Sanchis-Angulo, Y. Moliner-Martínez, P. Campíns-Falcó

Background

Silica materials vary widely in size, structure, and applicability, making their accurate characterization essential for ensuring proper performance across research and industrial applications. A strategy for hydrodynamic size assessment of silica materials ranging nanometers to micrometers is proposed here. Silica nanoparticles (SiO₂NPs) of different sizes, halloysite as silica nanotubes, and silica obtained from rice straw combustion residues have been characterized employing asymmetrical flow field flow fractionation technique in combination with a DLS detector (AF4-DLS). Additional analyses were performed using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), and batch-mode DLS.

Results

Firstly, the different silica materials were dispersed using alkaline treatment. For halloysite, a detailed dispersibility assay was performed using a wide variety of compounds to identify optimal conditions for stable suspensions. The sizes of SiO₂NPs obtained by AF4-DLS ranged between 15 and 200 nm, according to the type of NPs and their aggregation state. Halloysite exhibited sizes around 240–280 nm, corresponding to the transversal length. Additionally, the functionalization of this material with pigments was evaluated. As an example of micro material, silica extracted from combustion residues of rice straw was studied, resulting in average hydrodynamic diameters reaching up to 4 μm. Finally, analytical parameters were evaluated, and the results demonstrated suitable precision values, with limit of detection (LOD) in the range of 1.5∙10⁻⁴ % (w/v) to 7.2∙10⁻⁴ % (w/v).

Significance

These findings demonstrate the utility of the proposed AF4-DLS analytical strategy as an effective tool for silica characterization. By enabling assessment of hydrodynamic size across nanometer to micrometer scales, this approach enhances the understanding of particle behavior, aggregation, and functionalization, thereby supporting more informed decisions in the design and applications of silica materials.

二氧化硅材料在尺寸、结构和适用性方面差异很大，这使得它们的准确表征对于确保在研究和工业应用中的适当性能至关重要。本文提出了一种纳米至微米级二氧化硅材料的水动力尺寸评估策略。采用非对称流场流动分馏技术，结合DLS检测器（AF4-DLS），对不同粒径的二氧化硅纳米颗粒（SiO2NPs）、作为二氧化硅纳米管的高岭土以及从秸秆燃烧残渣中提取的二氧化硅进行了表征。使用扫描电子显微镜（SEM），傅里叶变换红外光谱（FTIR）和批量模式DLS进行其他分析。结果首先，对不同的二氧化硅材料进行碱性分散处理。对于高岭土，使用多种化合物进行了详细的分散性分析，以确定稳定悬浮液的最佳条件。根据NPs的类型和聚集状态的不同，AF4-DLS得到的SiO2NPs的尺寸在15 ~ 200 nm之间。埃洛石的尺寸约为240-280 nm，与横向长度相对应。此外，还对该材料与颜料的功能化进行了评价。以秸秆燃烧残渣中提取的二氧化硅为例，研究了其平均水动力直径可达4 μm。最后，对分析参数进行了评价，结果显示出合适的精密度值，检出限（LOD）在1.5∙10−4% （w/v）至7.2∙10−4% （w/v）之间。这些发现证明了AF4-DLS分析策略作为二氧化硅表征的有效工具的实用性。通过评估纳米到微米尺度的水动力尺寸，这种方法增强了对颗粒行为、聚集和功能化的理解，从而支持在设计和应用二氧化硅材料时做出更明智的决策。

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引用次数: 0

Synthetic cannabinoids in hair: a review of recent findings and analytical methods by LC-MS/MS 头发中合成大麻素：LC-MS/MS分析方法研究进展

IF 6 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-15 Epub Date: 2026-01-09 DOI: 10.1016/j.aca.2026.345078

Rafaela S. Pereira , Olívia B.O. Moreira , Marcone Augusto L. de Oliveira , Claudiane C. Canuto , Diogo O.C. Lemos , Lucas M. Duarte , Silvana V. Rodrigues

Background

Synthetic cannabinoids (SCs) represent a prominent class of new psychoactive substances (NPS), defined as substances of abuse that pose a significant public health threat. SCs are characterized by their structural diversity, high potency, and associated health risks. Their continuous emergence on the illicit drug market – driven by ongoing structural modifications – poses significant challenges for analytical detection, regulation, and toxicological evaluation. Hair analysis has proven to be a valuable biological matrix in forensic toxicology, offering an extended detection window and the ability to reflect chronic exposure.

Results

This critical review focused on the application of liquid chromatography coupled to mass spectrometry (LC-MS/MS) for the determination of SCs in hair. The most important steps in hair sample preparation – collection, segmentation, decontamination, pulverization, and extraction – are evaluated in depth. The advantages and limitations of both low-resolution and high-resolution mass spectrometry are discussed. Comprehensive tables summarize the main methodological parameters related to sample preparation and instrumental conditions.

Significance

Covering studies published between 2013 and 2025, this review presents an in-depth assessment of LC-MS/MS methodologies for SCs determination in hair, from sample preparation to instrumental optimization. It also provided an updated overview of SCs, considering nomenclature and toxicological effects. The findings underscore the pressing need for continued methodological advancements to improve SCs determination, supporting more accurate toxicological interpretations and providing new insights for forensic field.

背景：合成大麻素（SCs）是一类突出的新型精神活性物质（NPS），被定义为对公共卫生构成重大威胁的滥用物质。干细胞的特点是其结构多样性、高效能和相关的健康风险。它们在非法药物市场上不断出现——由持续的结构改变所驱动——对分析检测、监管和毒理学评价构成了重大挑战。毛发分析已被证明是法医毒理学中有价值的生物基质，提供了一个扩展的检测窗口和反映慢性暴露的能力。结果：本文综述了液相色谱-质谱联用技术（LC-MS/MS）在头发中SCs测定中的应用。在头发样品制备的最重要的步骤-收集，分割，去污，粉碎和提取-深度评估。讨论了低分辨率质谱和高分辨率质谱的优点和局限性。综合表格总结了与样品制备和仪器条件有关的主要方法参数。意义：本综述涵盖了2013年至2025年间发表的研究，从样品制备到仪器优化，对头发中SCs测定的LC-MS/MS方法进行了深入评估。它还提供了SCs的最新概述，考虑到命名和毒理学效应。这些发现强调了在方法上不断进步的迫切需要，以改善SCs的测定，支持更准确的毒理学解释，并为法医领域提供新的见解。

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引用次数: 0

Coreactant-accelerating electrochemiluminescence systems based on self-enhanced TiO2 inverse opal photonic crystals for ultrasensitive aptasensing of aflatoxin B1 in corn matrices with MoS2@Au/Pt nanocomposites as signal quencher 以MoS2@Au/Pt纳米复合材料作为信号淬灭剂，基于自增强TiO2逆蛋白石光子晶体的助反应加速电化学发光系统用于玉米基质中黄曲霉毒素B1的超灵敏感应

IF 6 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-15 Epub Date: 2026-01-23 DOI: 10.1016/j.aca.2026.345129

Zheng Xu, Jun Zhang, Shanshan Li, Maosen Zhao, Haijie Lu

Background

Aflatoxin B1 (AFB1), as the most toxic mycotoxin, has been classified into Group 1 type of carcinogen by WHO. Developing sensitive and accurate AFB1 detection methods for safeguarding food safety is extremely necessary. Photonic crystal (PhC)-based electrochemiluminescence (ECL) is an emerging biosensing technique with advantages of near-zero background and enhanced sensitivity. However, current PhC-based ECL biosensors are mainly focused on the enhancement of light scattering and electromagnetic field, with less attention paid to the coreactant acceleration. Therefore, it is of vital importance to develop PhC as coreactant accelerator for further research to increase the versatility of PhC-based ECL biosensors.

Results

Herein, we developed a coreactant-accelerating ECL system based on self-enhanced TiO₂ inverse opal photonic crystals (IO–TiO₂) for ultrasensitive determination of AFB1 with MoS₂@Au/Pt nanocomposites as signal quencher. IO-TiO₂ could act as the roles of ECL emitters and coreactant accelerators, which significantly enhances the ECL emission intensity. IO-TiO₂ fabricated with 300 nm polystyrene (PS) displayed the optimal ECL performances with pore size of inverse opal at 217 nm and current density at 0.60 A/m². MoS₂@Au/Pt, as the signal probe, could obviously quench the ECL signals due to high loading capacity of MoS₂ and broad-spectrum absorbance of Pt nanoparticles. When exposed to AFB1, DNA modified MoS₂@Au/Pt nanocomposites were detached from the electrode by the specific binding between AFB1 and its aptamer and the ECL intensity of IO-TiO₂ recovered. Under the optimized conditions, an ultrasensitive ECL biosensing platform for AFB1 monitoring was constructed with a detection of limit (LOD) of 3.3 pg/mL.

Significance

In the analysis of real corn matrices, the ECL biosensor exhibited good practicality with acceptable recoveries and RSDs for the measurement of AFB1. Combining the self-enhanced IO-TiO₂ emitters with coreactant-accelerating ECL systems, the biosensors demonstrated high sensitivity and selectivity, which opened new venue for the rational design of ECL biosensors and offered great opportunities in food safety analysis.

黄曲霉毒素B1 （AFB1）作为毒性最大的真菌毒素，已被世界卫生组织列为第一类致癌物。开发灵敏、准确的AFB1检测方法对于保障食品安全是十分必要的。基于光子晶体（PhC）的电化学发光（ECL）是一种新兴的生物传感技术，具有近零背景和灵敏度提高的优点。然而，目前基于phc的ECL生物传感器主要集中在光散射和电磁场增强上，对共反应物加速的关注较少。因此，开发PhC作为共反应物促进剂进行进一步研究，以提高PhC基ECL生物传感器的通用性具有重要意义。结果以MoS2@Au/Pt纳米复合材料为信号淬灭剂，建立了一种基于自增强TiO2逆蛋白石光子晶体（tio - TiO2）的共沉淀物加速ECL系统，用于AFB1的超灵敏检测。tio2可以作为ECL的发射体和共催化剂，显著增强了ECL的发射强度。用300 nm聚苯乙烯（PS）制备的tio2具有最佳的ECL性能，孔径为217 nm的反蛋白石，电流密度为0.60 A/m2。MoS2@Au/Pt作为信号探针，由于MoS2的高负载能力和Pt纳米粒子的广谱吸光度，可以明显地淬灭ECL信号。当AFB1暴露时，DNA修饰的MoS2@Au/Pt纳米复合材料通过AFB1与其适配体的特异性结合从电极上分离出来，并恢复了tio2的ECL强度。在优化条件下，构建了AFB1超灵敏ECL生物传感平台，检测限为3.3 pg/mL。在实际玉米基质分析中，ECL生物传感器具有良好的实用性，可用于测定AFB1的回收率和rsd。将自增强的IO-TiO2发射体与共反应加速ECL系统相结合，具有较高的灵敏度和选择性，为ECL生物传感器的合理设计开辟了新的领域，为食品安全分析提供了巨大的机遇。

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引用次数: 0

Molecular recognition-based affinity chromatography strategy for selective separation of cucurbit[5]uril and cucurbit[7]uril on hybrid monolithic materials 基于分子识别的亲和色谱策略在杂化单片材料上选择性分离葫芦[5]和葫芦[7]

IF 6.2 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-14 DOI: 10.1016/j.aca.2026.345404

Xiaolong Shen, Ruizhi Tang, Shujuan Ma, Yangyang Bian, Zichao Tang, Junjie Ou

引用次数: 0

Monitoring photochemical reactions catalyzed by nano-titanium dioxide using electrospray laser desorption ionization mass spectrometry 利用电喷雾激光解吸电离质谱法监测纳米二氧化钛催化的光化学反应

IF 6.2 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-14 DOI: 10.1016/j.aca.2026.345403

Min-Zong Huang, Hsin-Hui Liang, Chi-Yang Lee, Shu-Yao Lin, Chun-Mei Wu, Jentaie Shiea

引用次数: 0

A Colorimetric/Fluorescent/Electrochemical Tri-modal Biosensor Based on Dual CRISPR/Cas12a System for Detection of microRNA 基于CRISPR/Cas12a双系统的比色/荧光/电化学三模态生物传感器检测microRNA

IF 6.2 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-14 DOI: 10.1016/j.aca.2026.345393

Hehua Zhang, Huan Zhu, Hongmin Gao, Yang Zhou, Longbin Que, Shengzhong Rong, Hongkun Ma, Dong Chang, Hongzhi Pan

引用次数: 0

Systematic optimization of gel-free capillary zone electrophoresis for phosphodiester oligonucleotide separations at acidic pH 酸性条件下磷酸二酯寡核苷酸分离的无凝胶毛细管区带电泳系统优化

IF 6.2 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-14 DOI: 10.1016/j.aca.2026.345395

Jakob Haglöf, Julia Regnell, Cari E. Sänger-van de Griend

Background

Reliable analysis of oligonucleotides is essential for therapeutic development and biomarker studies, yet conventional methods often rely on gels or high-salt buffers that hinder mass spectrometry compatibility. MicroDNA and microRNA are commonly analyzed using liquid chromatography or capillary gel electrophoresis (CGE). In a recent study, we introduced a gel-free capillary zone electrophoresis (CZE) method for rapid, high-resolution separation of oligonucleotides at acidic pH.

Results

Here we optimized a gel-free capillary zone electrophoresis (CZE) method operating at acidic pH using a PVA-coated capillary and malonic acid-ammonia buffer. Adjustments to buffer composition, cation type, and temperature (up to 60 °C) enhanced resolution and reduced current, enabling rapid, high-resolution separation of phosphodiester oligonucleotides ranging from 18 to 25 nucleotides with excellent repeatability (<0.5% mobility variation).

Significance

This gel-free CZE approach provides a fast and reproducible platform, facilitating detailed characterization of phosphodiester oligonucleotides, microDNA, and microRNA in pharmaceutical and bioanalytical contexts.

可靠的寡核苷酸分析对于治疗开发和生物标志物研究至关重要，然而传统的方法往往依赖于凝胶或高盐缓冲液，这阻碍了质谱的兼容性。MicroDNA和microRNA通常使用液相色谱或毛细管凝胶电泳（CGE）进行分析。在最近的一项研究中，我们介绍了在酸性pH下快速、高分辨率分离寡核苷酸的无凝胶毛细管区带电泳（CZE）方法。结果我们优化了在酸性pH下使用pva包被毛细管和丙二酸-氨缓冲液的无凝胶毛细管区带电泳（CZE）方法。调整缓冲液组成、阳离子类型和温度（高达60°C）提高了分辨率，降低了电流，能够快速、高分辨率地分离磷酸二酯寡核苷酸，范围从18到25个核苷酸，具有出色的重复性（0.5%迁移率变化）。这种无凝胶CZE方法提供了一个快速和可重复的平台，便于在制药和生物分析环境中详细表征磷酸二酯寡核苷酸、微dna和微rna。

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引用次数: 0

Hydrangea-derived nitrogen-doped carbon dots: A dual-purpose platform for on-site chlortetracycline detection and time-limited anti-counterfeiting 绣球源氮掺杂碳点：现场检测和限时防伪的双重平台

IF 6.2 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-14 DOI: 10.1016/j.aca.2026.345398

Meiling Long, Decheng Peng, Jun Yang, Shaogui Wu

In this work, blue-emissive nitrogen-doped carbon dots (N-CDs) were prepared via a one-step hydrothermal method using Hydrangea macrophylla flowers as the carbon precursor and L-histidine as the nitrogen source, affording a quantum yield of 9.8%. The N-CDs emit bright blue fluorescence under 365 nm UV light but undergo self-quenching within 30 min. This “single-use luminescence” behavior is, to the best of our knowledge, exploited for anti-counterfeiting for the first time. When printed onto chiffon or cotton–linen textiles, the N-CDs generate non-toxic, washable, and non-reproducible “time-limited fluorescent identifiers.” In addition, the N-CDs exhibit an instantaneous response to chlortetracycline (CTC), showing fluorescence quenching at concentrations as low as 0.105 μmol L⁻¹ within a linear range of 20–75 μmol L⁻¹. The average recovery in rainwater samples approached 100%, outperforming most reported CD-based antibiotic probes. This study bridges two practical scenarios—environmental safety monitoring and wearable anti-counterfeiting—offering a green, low-cost, and scalable paradigm.

本研究以绣球花为碳前体，以l -组氨酸为氮源，采用一步水热法制备了蓝色发射氮掺杂碳点（N-CDs），产率为9.8%。N-CDs在365 nm紫外光下发出明亮的蓝色荧光，但在30 min内自猝灭。据我们所知，这种“一次性发光”的行为首次被用于防伪。当打印到雪纺或棉麻纺织品上时，n- cd产生无毒，可洗涤和不可复制的“限时荧光标识符”。此外，N-CDs对氯四环素（CTC）具有瞬时响应，在20 ~ 75 μmol L−1的线性范围内，当浓度低至0.105 μmol L−1时荧光猝灭。雨水样品的平均回收率接近100%，优于大多数报道的基于cd的抗生素探针。本研究结合了环境安全监测和可穿戴防伪两种实际场景，提供了一种绿色、低成本和可扩展的范例。

{"title":"Hydrangea-derived nitrogen-doped carbon dots: A dual-purpose platform for on-site chlortetracycline detection and time-limited anti-counterfeiting","authors":"Meiling Long, Decheng Peng, Jun Yang, Shaogui Wu","doi":"10.1016/j.aca.2026.345398","DOIUrl":"https://doi.org/10.1016/j.aca.2026.345398","url":null,"abstract":"In this work, blue-emissive nitrogen-doped carbon dots (N-CDs) were prepared via a one-step hydrothermal method using <em>Hydrangea macrophylla</em> flowers as the carbon precursor and L-histidine as the nitrogen source, affording a quantum yield of 9.8%. The N-CDs emit bright blue fluorescence under 365 nm UV light but undergo self-quenching within 30 min. This “single-use luminescence” behavior is, to the best of our knowledge, exploited for anti-counterfeiting for the first time. When printed onto chiffon or cotton–linen textiles, the N-CDs generate non-toxic, washable, and non-reproducible “time-limited fluorescent identifiers.” In addition, the N-CDs exhibit an instantaneous response to chlortetracycline (CTC), showing fluorescence quenching at concentrations as low as 0.105 μmol L<sup>−1</sup> within a linear range of 20–75 μmol L<sup>−1</sup>. The average recovery in rainwater samples approached 100%, outperforming most reported CD-based antibiotic probes. This study bridges two practical scenarios—environmental safety monitoring and wearable anti-counterfeiting—offering a green, low-cost, and scalable paradigm.","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"80 1","pages":"345398"},"PeriodicalIF":6.2,"publicationDate":"2026-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147465428","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Comparison of Solid Phase Microextraction Coatings for Headspace Extraction of Volatile Perfluoroalkyl Substances Using One-Dimensional and Comprehensive Two-Dimensional Gas Chromatography 一维和综合二维气相色谱法顶空萃取挥发性全氟烷基物质固相微萃取涂层的比较

IF 6.2 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-13 DOI: 10.1016/j.aca.2026.345389

Madison L. Williams, Aethena Fitzgerald, David Alonso, Joe Binkley, John Hayes, Michael Stebler, Emanuela Gionfriddo

引用次数: 0

Azetidination-based photocycloaddition enables regioisomer-resolved annotation of cholesteryl esters by negative-ion-mode LC-MS/MS 基于氮杂基的光环加成可以通过负离子模式LC-MS/MS对胆固醇酯进行区域异构体分辨注释

IF 6.2 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta

Pub Date : 2026-03-13 DOI: 10.1016/j.aca.2026.345392

Andrea Cerrato, Enrico Taglioni, Chiara Cavaliere, Aldo Laganà, Elena Lucà, Carmela Maria Montone, Anna Laura Capriotti

引用次数: 0

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