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Surface-doped Ru over WO3 nanocubes for highly selective and ppb-concentration 1-octen-3-ol sensing. 表面掺杂钌在WO3纳米立方体上的高选择性和ppb浓度1-辛烯-3-醇传感。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-02-01 Epub Date: 2025-09-30 DOI: 10.1016/j.talanta.2025.128933
Tingting Wang, Xinhua Zhao, Zhenxu Li, Yi Zhang, Zhu Zhang, Dachi Yang

The newly-emerged gas sensing detection of 1-octen-3-ol biomarker is expected to indirectly monitor foodborne illnesses caused by Salmonella-contaminated meat, which requires high selectivity and a ppb-concentration detection limit. Here, surface-doped ruthenium over tungsten oxide nanocubes (Ru/WO3 NCBs) have been synthesized by a wet-chemical approach for highly selective and ppb-concentration 1-octen-3-ol sensing. As-prepared Ru/WO3 NCBs exhibit a polycrystalline structure and consist of NCBs that have an average side length of ∼131 nm, and the Ru/WO3 NCBs show a high sensing response toward 5 ppm 1-octen-3-ol (Ra/Rg = 406), excellent selectivity, 50 ppb detection limit, 70 % relative humidity tolerance, and 54 days stability at 220 °C. The excellent sensing performance might be attributed to the electronic and chemical sensitization of Ru, which thickens the electron depletion layer and increases adsorbed oxygen to promote interfacial electron transfer and 1-octen-3-ol oxidation. Practically, Ru/WO3 NCBs have been integrated into a sensing device to simulate detecting 1-octen-3-ol, which has the potential for Salmonella detection in the future.

新出现的1-辛烯-3-醇生物标志物气敏检测有望间接监测沙门氏菌污染肉类引起的食源性疾病,该方法要求高选择性和ppb浓度检测限。本文采用湿化学方法合成了表面掺杂氧化钨纳米立方钌(Ru/WO3 NCBs),具有高选择性和ppb浓度1-辛烯-3-醇传感。制备的Ru/WO3 ncb表现出多晶结构,由平均边长为~ 131 nm的ncb组成,Ru/WO3 ncb对5 ppm的1-辛烯-3-醇(Ra/Rg = 406)具有高的传感响应,具有优异的选择性,50 ppb的检测限,70%的相对湿度耐受性,以及在220°C下54天的稳定性。优异的传感性能可能归因于Ru的电子和化学敏化作用,Ru增厚了电子耗尽层,增加了吸附氧,促进了界面电子转移和1-辛烯-3-醇氧化。实际上,Ru/WO3 ncb已经集成到传感装置中模拟检测1-辛烯-3-醇,这在未来有可能用于沙门氏菌检测。
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引用次数: 0
Generating a chemical database of organic nanomers and applying active learning to predict HOMO, LUMO and band gap: Accelerating optoelectronic nanopolymer materials discovery. 建立有机纳米化学数据库并应用主动学习预测HOMO、LUMO和带隙:加速光电纳米聚合物材料的发现。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-02-01 Epub Date: 2025-10-04 DOI: 10.1016/j.talanta.2025.128939
Qin Zhu, Yanwei Tang, Xinyao Ge, Chong Zhang, Xun Fu, Yongxia Wang, Dong Jin, Lizhu Dong, Jinyi Zhang, Qiang Zhao, Ying Wei, Xiaogang Cheng, Linghai Xie

Organic nanogrids are versatile molecular hornstones and nanoplatforms of organic high-dimensional, low-entropy materials. It is urgent to construct virtual databases of organic nanomers for accelerating the discovery and performance optimization of novel 0/1/2/3-dimensional nanopolymer optoelectronic materials. In this study, we generated a comprehensive dataset of 11,224 ladder-type gridarenes, covering a wide range of chemical compositions and structural variations. A random selection of 220 small sample sets was aggregated, and fragment-level constrained density functional theory (CDFT) was employed to extract molecular descriptors. These descriptors were then used to train machine learning models with high predictive accuracy for band gap, highest occupied molecular orbital (HOMO), and lowest unoccupied molecular orbital (LUMO) energies (the coefficient of determination values of 0.94, 0.92, and 0.87, respectively). During the active learning process, 3112 representative gridarenes were iteratively selected from our 11,224-compound library, refining band-gap predictions to a mean absolute error below 0.11 eV. This process pinpointed top candidates for blue-light emission and demonstrated an accelerated, data-driven route to next-generation organic optoelectronic nanomaterials.

有机纳米网格是有机高维、低熵材料的多用途分子角石和纳米平台。构建有机纳米虚拟数据库是加快新型0/1/2/3维纳米聚合物光电材料的发现和性能优化的迫切需要。在这项研究中,我们生成了一个包含11,224个阶梯型网格烯的综合数据集,涵盖了广泛的化学成分和结构变化。随机选取220个小样本集进行聚合,利用片段水平约束密度泛函理论(CDFT)提取分子描述符。然后使用这些描述符训练具有高预测精度的带隙、最高已占据分子轨道(HOMO)和最低未占据分子轨道(LUMO)能量的机器学习模型(决定系数分别为0.94、0.92和0.87)。在主动学习过程中,从我们的11,224个化合物库中迭代选择了3112个具有代表性的网格,将带隙预测的平均绝对误差提高到0.11 eV以下。这一过程确定了蓝光发射的最佳候选材料,并展示了下一代有机光电纳米材料的加速、数据驱动路线。
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引用次数: 0
Surface enhanced sharp-edged gold microneedles decorated on pencil graphitic microelectrode as efficient electrochemical sensing platform for sensitive detection of NADH in serum and urine samples. 铅笔型石墨微电极表面强化锐边金微针作为高效电化学传感平台,用于血清和尿液中NADH的灵敏检测。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-02-01 Epub Date: 2025-10-30 DOI: 10.1016/j.talanta.2025.129043
Mani Arivazhagan, Paramasivam Shanmugam, Samikannu Prabu, Rajaji Pavadai, Ganesha Honnu, Krishnamoorthy Shanmugaraj, Nagaraj Murugan, Yoong Ahm Kim, Jaroon Jakmunee

Accurate detection of NADH levels plays a critical role in the diagnosis and management of conditions ranging from metabolic disorders to neurodegenerative diseases such as Parkinson and Alzheimer. It also holds potential for therapeutic interventions targeting mitochondrial function and energy metabolism. Herein, we designed the miniaturized sharp-edged hyper-branched gold microneedles (Au MNDs) decorated with pencil graphitic microelectrodes (PGME) via single-step, green electrochemical deposition strategy in the absence of any redox mediators, organic solvents and enzymes, etc. The as-prepared Au microneedles demonstrate impressive direct electrocatalytic properties for NADH oxidation. Their sharp edges of the microneedles and the optimized transducers ionic mobility effectively enhance electrochemically active surface area and intrinsic charge transfer efficiency, making this electrode a powerful enzyme-mimic platform for detecting NADH. This morphology, combined with the unique surface features, fosters a highly ideal conditions for the rapid electron transfer from NADH to the Au MNDs @PGME. The nanostructures improve the mobility directly influences the speed and efficiency of electronic charge carriers, which accelerates the rate of electron transfer. This enhances the electrochemical kinetics of the system, contributing to rapid and sensitive detection of NADH. These attributes indicate that Au MNDs-modified microsensor holds great potential for high sensitivity (62.80 μA/μM cm-2), two distinct linear ranges: 0.1-4.5 μM and 4.5-54.5 μM, fast response (<2 s), and lower LOD for the reliable NADH detection. The miniaturized microsensors had a strong ability to prevent anti-interference from sensing of NADH. Notably, the current micro sensing platform, which is based on Au MNDs @PGME, has proven to be useful in clinical diagnostics by successfully testing for NADH sensing in human serum and urine samples in biomedical application.

准确检测NADH水平在从代谢紊乱到神经退行性疾病(如帕金森和阿尔茨海默病)的诊断和治疗中起着至关重要的作用。它还具有针对线粒体功能和能量代谢的治疗干预的潜力。本研究在不使用氧化还原介质、有机溶剂和酶等的情况下,采用单步绿色电化学沉积策略,设计了以铅笔石墨微电极(PGME)装饰的微缩尖边超支化金微针(Au MNDs)。所制备的金微针对NADH的氧化表现出令人印象深刻的直接电催化性能。微针的锋利边缘和优化的换能器离子迁移率有效地提高了电化学活性表面积和内在电荷转移效率,使该电极成为检测NADH的强大酶模拟平台。这种形态与独特的表面特征相结合,为从NADH到Au MNDs @PGME的快速电子转移提供了非常理想的条件。纳米结构的迁移率的提高直接影响电子载流子的速度和效率,从而加快了电子转移的速度。这增强了系统的电化学动力学,有助于快速和灵敏地检测NADH。这些特性表明,Au mnds修饰的微传感器具有高灵敏度(62.80 μA/μM cm-2)、0.1 ~ 4.5 μM和4.5 ~ 54.5 μM的线性范围、快速响应(
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引用次数: 0
Label-free Raman chemometric analysis for in situ authentication and molecular profiling of Wagyu beef under retail packaging. 无标签拉曼化学分析用于零售包装和牛的原位鉴定和分子分析。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-31 DOI: 10.1016/j.talanta.2026.129460
Jia-En Kao, Chang-Chun Li, Ming-Syue Lin, Kohei Yokosawa, Takakazu Nakabayashi, Tai-Sheng Yeh, Ian Liau

Wagyu beef's distinctive flavor and tenderness arise from its high levels of unsaturated intramuscular triglycerides. Although these compositional distinctions provide a unique Raman signature, extensive band overlap and background attenuation from packaging and frozen conditions hinder reliable in situ classification and constrain the interpretability of raw spectra. This study presents a label-free Raman spectroscopic and chemometric approach for authenticating Wagyu beef under realistic retail-like conditions. A supervised partial least squares discriminant analysis (PLS-DA) model was developed using spectra from unwrapped adipose tissue and evaluated with an independent validation set of frozen, plastic-wrapped samples from multiple breeds and suppliers. The model achieved 100% sample-level classification accuracy, supported by receiver operating characteristic and confusion-matrix analyses. To elucidate the molecular basis of discrimination and resolve spectral congestion, a two-stage decomposition combining singular value decomposition (SVD) and nonnegative matrix factorization (NMF) was applied, followed by nonnegative least squares (NNLS) fitting with pure triglyceride standards. The analyses yielded chemically interpretable components, revealing enrichment of unsaturated triglycerides in Wagyu beef consistent with established compositional data. To our knowledge, this is the first report applying Raman-based PLS-DA for Wagyu authentication and integrating SVD, NMF, and NNLS for molecular-level interpretation in food authentication. Overall, Raman spectroscopy integrated with interpretable spectral decomposition provides a rapid, nondestructive, and chemically transparent tool for meat authentication and quality assurance.

和牛的独特风味和嫩度源于其高水平的不饱和肌内甘油三酯。尽管这些成分差异提供了独特的拉曼特征,但由于包装和冷冻条件造成的广泛的波段重叠和背景衰减阻碍了可靠的原位分类,并限制了原始光谱的可解释性。本研究提出了一种无标签的拉曼光谱和化学计量学方法,用于在现实零售条件下验证和牛牛肉。利用未包裹脂肪组织的光谱建立了监督偏最小二乘判别分析(PLS-DA)模型,并使用来自多个品种和供应商的冷冻塑料包装样品的独立验证集进行评估。该模型在接收者工作特征和混淆矩阵分析的支持下实现了100%的样本级分类精度。为了阐明鉴别的分子基础和解决光谱拥挤问题,采用奇异值分解(SVD)和非负矩阵分解(NMF)相结合的两阶段分解方法,然后用纯甘油三酯标准进行非负最小二乘(NNLS)拟合。分析产生了化学可解释的成分,揭示了和牛牛肉中不饱和甘油三酯的富集与已建立的成分数据一致。据我们所知,这是第一次将基于拉曼的PLS-DA应用于和牛认证,并将SVD、NMF和NNLS集成在食品认证中进行分子水平解释。总的来说,拉曼光谱与可解释的光谱分解相结合,为肉类认证和质量保证提供了一种快速、无损和化学透明的工具。
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引用次数: 0
An antifouling electrochemical biosensor based on covalent organic framework-iridium nanocomposite functionalized with designed peptide for the detection of β-Amyloid in serum 基于设计肽功能化的共价有机骨架-铱纳米复合材料的防污电化学生物传感器用于血清中β-淀粉样蛋白的检测
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-31 DOI: 10.1016/j.talanta.2026.129483
Wenqing Wang , Baoping Zhu , Shujie Cheng , Rui Han , Min Chen , Xiliang Luo
Alzheimer's disease (AD) is a neurodegenerative disorder closely associated with the aggregation of β-Amyloid (Aβ) peptides, particularly Aβ 1–42. Electrochemical biosensors hold great potential for serological Aβ 1–42 detection due to their high sensitivity and rapid response capability. However, their performances in complex matrices such as serum are compromised by biofouling and signal interference. The biosensors with functional peptide-modified interfaces, leveraging Ir–S coordination, have had improved antifouling performance and stability. Nevertheless, conventional iridium nanoparticle (IrNPs) electrodeposition often yields heterogeneous structures with poor uniformity, limiting the consistency and sensitivity of such platforms. To address this, we developed an innovative electrochemical biosensor based on a covalent organic framework (COF)-mediated interface. Using TpPa-1 COF (Tp: 1,3,5-triformylphloroglucinol; Pa: p-phenylenediamine) as a structural template, we achieved uniform and high-density loading of IrNPs (IrNPs@COF). The functional peptides were subsequently assembled via robust Ir–S coordination, creating a synergistic antifouling sensing platform. This biosensor enables ultrasensitive and selective detection of Aβ 1–42 in serum, demonstrating significant potential for reliable early diagnosis of AD.
阿尔茨海默病(AD)是一种与β-淀粉样蛋白(a β)肽聚集密切相关的神经退行性疾病,特别是a β 1-42。电化学生物传感器具有灵敏度高、反应速度快的特点,在血清学中检测Aβ 1-42具有很大的潜力。然而,它们在复杂基质(如血清)中的性能受到生物污垢和信号干扰的影响。具有功能性肽修饰界面的生物传感器,利用Ir-S配位,具有更好的防污性能和稳定性。然而,传统的铱纳米颗粒(IrNPs)电沉积通常会产生均匀性差的非均质结构,限制了这种平台的一致性和灵敏度。为了解决这个问题,我们开发了一种基于共价有机框架(COF)介导界面的创新电化学生物传感器。使用TpPa-1 COF (Tp: 1,3,5-三甲酰间苯三醇;Pa:对苯二胺)作为结构模板,我们实现了IrNPs的均匀高密度加载(IrNPs@COF)。功能肽随后通过强大的Ir-S配位组装,创建一个协同的防污传感平台。这种生物传感器能够超灵敏和选择性地检测血清中的β 1-42,显示出可靠的阿尔茨海默病早期诊断的巨大潜力。
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引用次数: 0
Rapid urine screening and staging of chronic kidney disease via NAD(P)H-activated dual-salt fluorescent probe. 通过NAD(P) h激活双盐荧光探针快速筛查和分期慢性肾脏疾病。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-31 DOI: 10.1016/j.talanta.2026.129470
Yanbo Li, Guyan Duan, Hua Xiao, Deyang Xi, Liqiang Zhu, Longhua Guo, Bohan Liu, Jianbo Wang, Ya Liu, Mingxi Fang

Chronic kidney disease (CKD) requires fast, noninvasive tools for early detection and staging that go beyond conventional serum creatinine/eGFR measurements. NAD(P)H, a key coenzyme in cellular metabolism, energy transfer, and redox signaling, is closely associated with the normal kidney function. Monitoring intracellular NAD(P)H levels offers a promising strategy for CKD assessment. Here, we present a novel dual-salt fluorescent probe (CKD-pro) for the rapid and sensitive detection of NAD(P)H. The CKD-pro is constructed from 1-methylquinolinium and naphthalene thiazolium salt units connected through vinyl linkers. Upon reduction of the quinolinium moiety by NAD(P)H, the probe converts into a donor-π-acceptor (D-π-A) architecture, resulting in a rapid fluorescence signal at 585 nm. Probe exhibits excellent analytical performance, with a linear response over 0-2 μM, a limit of detection (LOD) of 20 nM, and a response time shorter than 2 min. It also shows high selectivity and good biocompatibility, enabling real-time monitoring of NAD(P)H dynamics in G6PD-knockout cancer cells and HK-2 renal cells under hypoxia. In a clinical proof-of-concept study (midstream urine, n = 30 CKD patients and n = 10 healthy controls), the fluorescence signal from CKD-pro was significantly higher in CKD patients, showed an inverse correlation with eGFR, and successfully discriminated CKD from healthy individuals (AUC = 0.847). Moreover, the probe effectively stratified mild-to-moderate (stages 1-3) and severe (stages 4-5) CKD with an AUC of 0.915. Together, these findings establish CKD-pro as the first urine-based optical NAD(P)H probe for non-invasive CKD screening and staging, underscoring its clinical translation potential.

慢性肾脏疾病(CKD)需要快速、无创的工具来进行早期检测和分期,而不仅仅是传统的血清肌酐/eGFR测量。NAD(P)H是细胞代谢、能量传递和氧化还原信号传导的关键辅酶,与正常肾功能密切相关。监测细胞内NAD(P)H水平为CKD评估提供了一种有希望的策略。在此,我们提出了一种新的双盐荧光探针(CKD-pro),用于快速灵敏地检测NAD(P)H。CKD-pro由1-甲基喹啉和萘噻唑盐单元通过乙烯基连接剂连接而成。在NAD(P)H还原喹啉基团后,探针转变为供体-π-受体(D-π-A)结构,在585 nm处产生快速荧光信号。探针具有良好的分析性能,线性响应大于0-2 μM,检出限(LOD)为20 nM,响应时间小于2 min。它还具有高选择性和良好的生物相容性,可以实时监测缺氧条件下g6pd敲除癌细胞和HK-2肾细胞中的NAD(P)H动态。在一项临床概念验证研究(中程尿液,n = 30名CKD患者和n = 10名健康对照)中,CKD-pro的荧光信号在CKD患者中显著升高,与eGFR呈负相关,成功区分CKD与健康个体(AUC = 0.847)。此外,探针有效地分层轻度至中度(1-3期)和重度(4-5期)CKD, AUC为0.915。总之,这些发现确立了CKD-pro作为首个基于尿液的光学NAD(P)H探针,用于无创CKD筛查和分期,强调了其临床转化潜力。
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引用次数: 0
A nanosensor platform for cell gene transfection and single-cell nanovibration dynamic monitoring. 用于细胞基因转染和单细胞纳米振动动态监测的纳米传感器平台。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-30 DOI: 10.1016/j.talanta.2026.129486
Zhen Zhen Xu, Yongjia Wang, Fei Fei, Juan Li, Han Yan

Cell transfection and dynamic monitoring of subsequent cellular physiological activity play a crucial role in studying gene function and regulating gene expression. However, platforms integrating cell transfection with dynamic monitoring of cellular physiological activity are rarely reported. Here, we propose a novel technology using a nanopore array platform combined with nanodrums fabricated from ultrathin graphene, which enables single-cell transfection while dynamically monitoring post-transfection changes in cellular physiological activity. In our exploration, we found that random oscillation amplitudes generated by single OCI-Ly3 cells reached up to ∼20 nm. After transfection with the ME2 gene knockdown sequence (shME2), cellular physiological activity was inhibited, and the random oscillations were suppressed, with amplitudes decreasing to < 5 nm. Our results provide a high-throughput potential and efficient approach for gene transfection and dynamic monitoring of cellular physiological activity, offering valuable insights for cell-based drug screening, cancer cell subtype classification, and other applications.

细胞转染及后续细胞生理活动的动态监测在研究基因功能和调控基因表达中起着至关重要的作用。然而,结合细胞转染和细胞生理活动动态监测的平台鲜有报道。在这里,我们提出了一种使用纳米孔阵列平台结合超薄石墨烯纳米鼓的新技术,该技术可以在单细胞转染的同时动态监测转染后细胞生理活性的变化。在我们的探索中,我们发现单个OCI-Ly3细胞产生的随机振荡幅度可达~ 20 nm。ME2基因敲低序列(shME2)转染后,细胞生理活性受到抑制,随机振荡受到抑制,振幅减小至
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引用次数: 0
Organic electrochemical transistors (OECT) based biosensors for the detection of small molecule metabolites. 基于有机电化学晶体管(OECT)的小分子代谢物检测生物传感器。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-30 DOI: 10.1016/j.talanta.2026.129487
Md Maruf Ahmed, Jiahong Xiang, Dhamodharan Arumugam, Zonish Zeb, Qin Xu

Recently, organic electrochemical transistors (OECTs) have emerged as robust platforms for chemical and biological sensing, due to their intrinsic signal amplification, biocompatibility, and low-voltage functionality. OECTs have exhibited tremendous promise for detecting small molecule metabolites (SMMs), which are crucial as biomarkers in medical diagnosis, environmental surveillance, and food quality monitoring. This review provides an in-depth analysis of recent advancements in OECT-based sensing devices for the detection of SMMs. Besides, the fundamental design concepts of OECTs, device structures, choice of materials, and functionalization techniques are studied to enhance selectivity and sensitivity. The incorporation of recognition elements-such as enzymes, aptamers, and molecularly imprinted polymers-on the gate or channel to facilitate target-specific interactions has been studied. Furthermore, the significance of channel engineering, microfluidic integration, and nanomaterial inclusion in improving device performance has also been discussed. The review highlights the main obstacles that impede the extensive development of OECTs, including baseline drift, signal instability, and selectivity. Finally, future prospects are explored, emphasizing rising trends in smart materials, micro platforms, and wearable diagnosis. This study seeks to assist researchers in creating next-generation OECT sensors designed for real-time, selective, and sensitive identification of SMMs.

近年来,有机电化学晶体管(OECTs)因其固有的信号放大、生物相容性和低电压功能而成为化学和生物传感的强大平台。oect在检测小分子代谢物(SMMs)方面显示出巨大的前景,这些代谢物在医学诊断、环境监测和食品质量监测中作为生物标志物至关重要。这篇综述提供了一个深入的分析,最近的进展,基于oect传感装置检测smm。此外,研究了OECTs的基本设计概念、器件结构、材料选择和功能化技术,以提高选择性和灵敏度。已经研究了识别元件(如酶、适体和分子印迹聚合物)在门或通道上的结合,以促进目标特异性相互作用。此外,还讨论了通道工程、微流控集成和纳米材料在提高器件性能方面的意义。这篇综述强调了阻碍oect广泛发展的主要障碍,包括基线漂移、信号不稳定和选择性。最后,展望未来,强调智能材料、微平台和可穿戴诊断的发展趋势。本研究旨在帮助研究人员创建下一代OECT传感器,用于实时、选择性和敏感地识别smm。
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引用次数: 0
Microstructured substrate based on in situ growth of silver particles for copper determination in liquid samples by LIBS. 基于原位生长银颗粒的微结构衬底液相色谱法测定液体样品中的铜。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-30 DOI: 10.1016/j.talanta.2026.129465
Nilvan A Silva, Ivo M Raimundo, Maria Clara M de Andrade, Fernanda K da Silva, André Galembeck

The development of simple and efficient analytical methods is fundamental for controlling the levels of toxic metals in liquid samples. In the present study, it is proposed the fabrication of a microstructured substrate based on filter paper, using in situ growth method of silver nanoparticles (AgNPs) into silver microparticles (AgMPs) to enhance the LIBS emission signal in the determination of Cu(II) in different liquid samples. Initially, ascorbic acid, NaBH4 and SnCl2 were evaluated as reducing agents for Ag particle formation. An 8-fold improvement in the copper signal was obtained when SnCl2 was used. The Ag particles obtained with the latter reducing agent were further grown, and the signal was enhanced up to 14-fold compared to the traditional LIBS method using unmodified filter paper. UV-Vis diffuse reflectance spectroscopy, X-ray diffraction measurements, and scanning electron microscopy (SEM) indicated efficient immobilization of both Ag nano- and microparticles on the microfibers of substrate. A calibration analytical curve for Cu(II) ions was obtained with a coefficient of determination (R2) of 0.99, a linear response from 0.2 to 1.0 mg L-1, and LOD and LOQ of 34 and 114 μg L-1, respectively. The signal enhancement achieved with the microstructured substrate fabricated using the in situ growth method can be attributed to the synergistic effect of the nanostructures present in the cellulosic microfibers and the surface enhancement caused by the dense layer of Ag microparticles. The developed analytical strategy was successfully applied to the determination of Cu(II) ions in fortified samples of river water, artificial urine, tea infusion, and canned tea, providing recoveries ranging from 85 to 112 %. These results indicate the effectiveness of a microstructured silver substrate for sensitive detection of metal ions at low concentrations in liquid samples.

开发简单有效的分析方法是控制液体样品中有毒金属含量的基础。在本研究中,提出了一种基于滤纸的微结构衬底,利用原位生长的方法将银纳米粒子(AgNPs)生长成银微粒(AgMPs),以增强LIBS发射信号,用于测定不同液体样品中的Cu(II)。最初,抗坏血酸、NaBH4和SnCl2被评估为银颗粒形成的还原剂。当使用SnCl2时,铜信号得到了8倍的改善。后一种还原剂得到的Ag颗粒进一步生长,与使用未改性滤纸的传统LIBS方法相比,信号增强了14倍。紫外可见漫反射光谱、x射线衍射测量和扫描电镜(SEM)表明,纳米和微颗粒Ag都有效地固定在衬底的微纤维上。建立了Cu(II)离子的校正分析曲线,其决定系数(R2)为0.99,线性响应范围为0.2 ~ 1.0 mg L-1,定量限和定量限分别为34和114 μg L-1。使用原位生长方法制备的微结构衬底实现的信号增强可归因于纤维素微纤维中存在的纳米结构和银微粒致密层引起的表面增强的协同效应。所建立的分析策略成功地应用于河水、人工尿液、茶叶冲剂和罐装茶强化样品中Cu(II)离子的测定,其回收率为85% ~ 112%。这些结果表明微结构银衬底对液体样品中低浓度金属离子的灵敏检测是有效的。
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引用次数: 0
Incorporating cIMS in an analytical framework for the in-depth characterization of food triacylglycerols. 将cIMS纳入深入表征食品甘油三酯的分析框架。
IF 6.1 1区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-30 DOI: 10.1016/j.talanta.2026.129489
Carlo Roberto de Bruin, Wouter J C de Bruijn, Bram van de Put, Jean-Paul Vincken, Marie Hennebelle

Characterization of the triacylglycerol (TAG) composition of food oils is challenging, in particular due to the presence of isomers. The main bottleneck is the incomplete separation of isomeric TAGs in liquid chromatography coupled to mass spectrometry (LC-MS), hindering identification because of mixed fragmentation spectra. In this study, the potential of adding cyclic ion mobility spectrometry (cIMS) as an additional dimension of separation in LC-MS analysis of food oils was explored to improve TAG isomer characterization. An analytical framework was created to achieve TAG isomer characterization by combining gas chromatography-MS (GC-MS), LC-MS, and cIMS-MS. TAG standards were used to evaluate the best option(s) for TAG isomer identification: fragmentation ratios, which can only be determined from pure fragmentation spectra obtained after separation of isomers in cIMS-MS; collisional cross section (cIMSCCSN2) values; or a combination thereof. Fragmentation ratios from pure fragmentation spectra yielded the strongest approach for isomer identification, as some TAG isomers were too close in cIMSCCSN2 for confident identification. Finally, using this framework, we identified 21 TAG isomers in sunflower and olive oils, 11 of which would not have been identified without the use of cIMS-MS. Overall, this study demonstrates the potential of the extra separation dimension provided by cIMS and its complementarity with classical GC- and LC-MS analyses.

表征食用油的三酰基甘油(TAG)组成具有挑战性,特别是由于其异构体的存在。主要的瓶颈是液相色谱-质谱(LC-MS)中异构标签的分离不完全,由于碎片化光谱的混合,阻碍了鉴定。本研究探讨了在LC-MS分析中加入环离子迁移谱(cIMS)作为额外分离维度的潜力,以改善TAG异构体的表征。通过气相色谱-质谱(GC-MS)、LC-MS和cIMS-MS相结合,建立了一个分析框架来实现TAG异构体的表征。使用TAG标准来评估鉴定TAG异构体的最佳选择:破碎率,这只能通过cIMS-MS分离异构体后获得的纯破碎光谱来确定;碰撞截面(cIMSCCSN2)值;或者两者的组合。纯碎片化光谱的碎片化比率是鉴定异构体的最有效方法,因为在cIMSCCSN2中,一些TAG异构体太接近,无法进行可靠的鉴定。最后,利用这一框架,我们鉴定了向日葵和橄榄油中的21种TAG异构体,其中11种如果不使用cIMS-MS是无法鉴定的。总的来说,本研究证明了cIMS提供的额外分离维度的潜力,以及它与经典的气相色谱和LC-MS分析的互补。
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