Analytical Methods最新文献

{"title":"A protein-nanoparticle conjugate platform for simplified and sensitive protease activity assays.","authors":"Masafumi Sakono, Kazuki Higashi, Mitsuki Nakamura, Naomi Sakono","doi":"10.1039/d5ay01006c","DOIUrl":"https://doi.org/10.1039/d5ay01006c","url":null,"abstract":"<p><p>Gold nanoparticles (AuNPs) have attracted increasing attention as functional platforms for biosensing due to their high biocompatibility and tunable surface properties. In this study, we developed a protease activity assay using NanoLuc luciferase (NLuc) as a luminescent reporter, genetically fused to a gold-binding peptide (AuBP1) and a TEV protease (TEVp) recognition sequence. The fusion proteins were immobilized onto AuNPs <i>via</i> the gold-binding peptide. Upon TEVp treatment, NLuc was cleaved and released from the AuNP surface, resulting in a measurable increase in luminescence intensity. Two measurement strategies were evaluated: one involving centrifugation-based separation after cleavage, and another without separation. The separation method showed a broader dynamic range and higher sensitivity, while the non-separation method enabled a simplified workflow with sufficient luminescence response. The results demonstrate the feasibility of combining recombinant protein technology with AuNPs to construct functional biosensors for protease assays. This approach may offer a practical and adaptable tool for further development in bioanalytical applications.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144681688","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Compositional analysis of archaeological leather and simulated leather and their degradation research based on HRMS.","authors":"Xihe Yang, Yizhu Liu, Zhenzhuo Liu, Jingxuan Liu, Jiahang Song, Yang Zhou, Yanli Cui","doi":"10.1039/d5ay00665a","DOIUrl":"https://doi.org/10.1039/d5ay00665a","url":null,"abstract":"<p><p>Leather, one of the earliest natural materials, was extensively used not only in daily attire but also in military protection in ancient times. Combined with simulated degradation experiments, high-resolution mass spectrometry (HRMS) was employed for the rapid and non-targeted detection of components in archaeological leathers, and for the systematic analysis of the chemical composition of leather samples. Comparative amino acid analysis of simulated and archaeological leather samples demonstrated that the L-hydroxyproline content and the signal intensity ratio of isoleucine and leucine to valine serve as integrated parameters for evaluating the aging status of leather. Moreover, the identification of other amino acids and tens of degraded products such as succinic acid, L-carnitine and 4-guanidinobutanoic acid deserve special attention. 4-Guanidinobutanoic acid existed in both simulated leather and archaeological artifacts. This research provides a new analytical tool for gaining significant insights into ancient leathers and their degradation status. In addition, HRMS enables the detection of early degradation signals in cultural relics, allowing conservation professionals to quantify degradation levels among different artifacts. This facilitates the prioritization of deteriorated leathers by heritage institutions.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144681690","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Perovskite nanocrystals@covalent organic framework as a nanothermometer for sensitive temperature sensing.","authors":"Huijun Liang, Xinyu Wang, Hongjun Chen","doi":"10.1039/d5ay00891c","DOIUrl":"https://doi.org/10.1039/d5ay00891c","url":null,"abstract":"<p><p>Perovskite nanocrystal-based temperature sensors have drawn extensive attention. Improving the photostability of perovskites and their sensitivity to temperature are urgent issues that need to be addressed. Herein, a nanothermometer for color-changing temperature indicators is designed based on perovskite nanocrystals encapsulated in a covalent organic framework (CsPbBr₃ NCs@COF-V). Different temperature-response fluorescence behaviors originate from the photoluminescence of CsPbBr₃ NCs at 522 nm. CsPbBr₃ NCs@COF-V achieves temperature sensing in the range of 20-89 °C and shows high potential as a thermometer for monitoring the body temperature. Significantly, spherical COF-V boosts fluorescence stability, fluorescence lifetime, and sensitivity to temperature of CsPbBr₃ NCs.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144688354","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comprehensive quality evaluation of Codonopsis Radix using HPLC fingerprinting, quantitative analysis, and chemometrics analysis.","authors":"Jieyu Lei, Rulan Jiang, Meihui Gong, Huimin Wu, Wenli Chen, Xinjun Xu","doi":"10.1039/d5ay00471c","DOIUrl":"https://doi.org/10.1039/d5ay00471c","url":null,"abstract":"<p><p>Codonopsis Radix (CR), a traditional Chinese medicine with significant medicinal value, has been widely used for many years. In this study, a comprehensive quality evaluation system for CR from different regions was established using high-performance liquid chromatography (HPLC). First, the optimal extraction conditions for two glycoside components from CR were determined through response surface methodology, with the following parameters: a methanol ratio of 80%, an extraction time of 35 min, and a liquid-to-solid ratio of 50 : 1. This optimized extraction method was applied to both fingerprinting and quantitative analysis. In the quantitative analysis, the calibration curves exhibited excellent linearity (<i>R</i>² ≥ 0.9998) within the tested range, and the mean recoveries ranged from 99.46% to 101.51%. A common fingerprint, consisting of 13 characteristic peaks, was established for CR samples from different production areas in China. HPLC-DAD-ESI-MS/MS was used to further identify the common peaks in the fingerprint. Various chemometrics analyses, including similarity analysis (SA), hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares discriminant analysis (OPLS-DA), were employed to classify the samples. Among these methods, OPLS-DA was particularly effective in distinguishing CR samples of different plant sources. The results demonstrate that the established method is effective for the comprehensive quality evaluation of CR, providing a reliable approach for its quality control and standardization.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144681691","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comparative analysis of hyperspectral and near-infrared spectroscopy for bloodstain deposition time estimation.","authors":"Ying Liang, Qifu Yang, Jiaquan Wu, Kun Ma, Xinyu Zhang, Huihui Ren, Hanyu Zhu, Xingshuai Peng, Jiateng Wang, Jianqiang Zhang","doi":"10.1039/d4ay02167c","DOIUrl":"https://doi.org/10.1039/d4ay02167c","url":null,"abstract":"<p><strong>Background: </strong>Bloodstains are a prevalent and critical type of forensic evidence at crime scenes. Accurate determination of bloodstain age is essential for crime resolution, and non-destructive spectral methods are instrumental in this process. While extensive research has established the practicality of hyperspectral imaging (HSI) in specific forensic contexts, limited studies have explored near-infrared (NIR) spectroscopy. Owing to its superior penetration capabilities and high sensitivity, NIR holds promise in addressing certain limitations of HSI. This study aims to assess the applicability of NIR spectroscopy for bloodstain age estimation in forensic contexts and to compare its efficacy with HSI.</p><p><strong>Results: </strong>Bloodstains were aged on various substrates over a 60 day period, with periodic analyses conducted using both spectral methods. Chemometric analysis of the spectral data was performed following SNV preprocessing and application of different regression algorithms. First, linear regression analysis was utilized to determine the effect of material on bloodstain deposition. Under the premise of distinguishing materials, partial least squares (PLS) regression was employed to extract eight latent variables from HSI and NIR spectral data for regression prediction. However, the prediction performance was suboptimal. To address this, polynomial features were introduced into the PLS regression algorithm to capture the nonlinear relationships in the spectral data, and the improved model significantly enhanced the prediction performance. Furthermore, PLS polynomial regression was applied to predict homologous data, and the results also demonstrated favorable performance. Finally, to optimize the prediction accuracy of multimodal data, a multilayer perceptron (MLP) was introduced for regression prediction through multimodal data fusion, further improving the overall performance of the model. Finally, predictive performance was evaluated across models, emphasizing their specific strengths. For homologous data fusion, comparable root mean square errors of prediction (RMSEP) were achieved for HSI and NIR spectra, at 8.35 and 8.15 days, respectively. Similar RMSEP values were observed in multimodal data fusion, and the accuracy of both low-level and intermediate-level fusion methods was evaluated.</p><p><strong>Significance: </strong>HSI and NIR spectroscopy each provide unique advantages in bloodstain detection. Data fusion of these methods helps mitigate external influences, enhancing the approach's general applicability. This integrated method facilitates rapid estimation of bloodstain age at crime scenes, aiding in crime timeline determination and presenting valuable potential for forensic applications.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144681689","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development of a natural product-based selective fluorescent sensor for Cu²⁺ and DNA/protein: insights from docking, DFT, cellular imaging and anticancer activity.","authors":"Sourav Pakrashy, Manik Das, Sounik Manna, Sujata Maiti Choudhury, Hazeena Shinziya, Bhriguram Das, Malay Dolai, Avijit Kumar Das","doi":"10.1039/d5ay00778j","DOIUrl":"https://doi.org/10.1039/d5ay00778j","url":null,"abstract":"<p><p>The natural product seselin (SS), was synthesized and characterized spectroscopically for the selective detection of Cu²⁺ and biomolecules such as ct-DNA and BSA. The probe exhibits strong bluish emission in a MeOH-H₂O (7 : 3, v/v) HEPES buffer solution (pH 7.4) at 453 nm. Upon exposure to Cu²⁺, the SS solution shows a selective fluorescence 'turn-off' with a binding constant of 2.13 × 10⁵ M^-1 and a detection limit of 3.48 × 10^-8 M. The HOMO-LUMO energy gap of the probe SS decreases from Δ<i>E</i> = 7.97 eV to Δ<i>E</i> = 7.77 eV upon binding with Cu²⁺, indicating enhanced stability due to ligand-metal complex formation. Significantly, the ligand SS exhibits fluorescence enhancement in the presence of ct-DNA and BSA, resulting in a visible fluorescence change from colorless to blue, with binding constants of 4.8 × 10⁴ M^-1 and 4.7 × 10⁴ M^-1, respectively. The binding interactions of SS with biomacromolecules have been explored through molecular docking studies, revealing that the probe can serve as a promising anti-cancer and anti-viral agent. Furthermore, the probe SS demonstrates potent anticancer activity in treatments involving MCF-7 and HLC cells. Additionally, the probe SS is capable of detecting intracellular Cu²⁺ in live MCF-7 cell lines.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144673388","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of polycyclic aromatic hydrocarbons in distilled beverages using HPLC-DAD as a proof of concept for dispersive droplet extraction and <i>in situ</i> formation of magnetic ionic liquids.","authors":"Camila Will, Lucas Morés, Gabrieli Bernardi, Jared L Anderson, Eduardo Carasek","doi":"10.1039/d5ay00078e","DOIUrl":"https://doi.org/10.1039/d5ay00078e","url":null,"abstract":"<p><p>Polycyclic aromatic hydrocarbons (PAHs) are a class of compounds known for their genotoxic and carcinogenic effects. They can be formed by the pyrolysis of organic matter and can be present in several matrices, including distilled beverages. Since these samples also contain different interferents and low concentrations of these analytes, it is important that a sample preparation step be performed prior to analysis. Although many methods have been reported for the analysis of these analytes, only a few have explored alternative procedures and extraction materials, such as the use of magnetic ionic liquids (MILs) and microextraction approaches. The development of alternative extraction techniques can improve analytical figures of merit and sample throughput, while also enhancing analyst safety. In this work, two <i>in situ</i> formed MILs, [Co(C₄IM)₄][NTf₂]₂ and [Ni(C₄IM)₄][NTf₂]₂, were employed as extraction phases for the high-throughput parallel dispersive droplet extraction (Pa-DDE) of PAHs in distilled beverages such as cachaça and rum. In this approach, a 96-well plate system with magnets was used to collect the MIL formed during the extraction. This permitted up to 96 samples to be processed simultaneously, resulting in sample preparation times of less than 1 minute per sample when using the optimized procedure. Besides extraction time, the type and amount of MILs were evaluated and optimum conditions were obtained using 10 mg of [Co(C₄IM)₄]Cl₂. Limits of detection (LOD) and quantification (LOQ) ranged from 0.3 to 7.5 μg L^-1 and 1 to 25 μg L^-1, respectively. All values for determination coefficients were higher than 0.991 and were considered adequate. The values of intraday and interday precision were all lower than 20.8 and 26.2%, respectively. Finally, accuracy was evaluated after relative recovery studies performed with 5 samples and varied from 52.1 to 150.1%. Samples used for this study were evaluated and none of the analytes were detected. This work represents a new application of <i>in situ</i> formed MILs for the analysis of more complex samples, since most of the previous studies using this extraction phase were evaluated in water samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144673387","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Isolation and detection of target cells in blood <i>via</i> immunomagnetic separation and atomic emission spectroscopy.","authors":"McKenna M McKay, Kensington H Fansler, Ke Liu, Dimitri Pappas","doi":"10.1039/d5ay00937e","DOIUrl":"https://doi.org/10.1039/d5ay00937e","url":null,"abstract":"<p><p>The identification and quantification of cells in blood can serve to inform disease diagnosis and prognosis for patients. However, sample complexity presents a challenge for achieving sensitive and specific detection methods. Furthermore, there is a need to alleviate current standard clinical protocols from operator burden, limit the required sample volumes, and to reduce analysis timescales, all while maintaining sensitivity. This study presents a novel atomic emission cytometry assay for the detection of cells in blood with high specificity and sensitivity (LOD = 84 cells per μL), requiring only 500 μL sample volume and 1 hour of combined processing and analysis time, exhibiting the potential for broad applications in disease diagnosis. Metal nanoparticles equipped with antibodies serve as a targeted cell labeling platform, as well as an integrated method for immunomagnetic separation and subsequent quantification <i>via</i> microwave plasma-atomic emission spectroscopy (MP-AES) analysis. This assay can also be modified to include multiple types of metal-based nanoparticles and/or target multiple cell surface markers for simultaneous detection of different cell populations within the same sample. The simplicity, specificity, and efficiency of this assay mark it as a viable integrated diagnostic platform for cellular-based disease diagnosis.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144657827","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Sustainability from the start: biochar-based conductive inks enable the streamlined fabrication of green electroanalytical devices.","authors":"Florencia Bernassani, Monica Mosquera-Ortega, Ismael Sánchez, Sabina Susmel, Eduardo Cortón, Federico Figueredo","doi":"10.1039/d5ay00740b","DOIUrl":"https://doi.org/10.1039/d5ay00740b","url":null,"abstract":"<p><p>The design of low-cost and disposable printed electrodes (PEs) has garnered significant attention from the scientific community in recent years. It is crucial to achieve industrial scalability by addressing the cost of conductive inks and ensuring their environmentally friendly disposal. The utilization of biochar, a carbon-rich material derived from the pyrolysis of biomass waste, represents a promising and sustainable alternative to conventional carbon sources. In this study, peanut shell biochar produced with a low-cost pyrolytic kiln reactor was incorporated into conductive inks. As far as we know, biochar-based ink was used to fully fabricate stencil-printed electrodes for the first time. Three different chemical treatments were employed to activate the biochar and enhance its properties. XPS analysis and electrochemical characterization studies showed that organic solvents improved the characteristics of the biochar when compared to acid or alkaline activation treatments. As a proof of concept, the electrodes were used to detect paracetamol as a model analyte for emerging environmental contaminants. An analytical greenness metric (AGREE) was used to infer how environmentally friendly the analytical procedure is, yielding an overall score of 0.72, which indicates a high degree of environmental sustainability. This study underscores the importance of implementing simple strategies to obtain cost-effective PE, thereby promoting green analytical methods using recycled materials such as bio-waste-derived biochar. This approach may reduce dependence on non-environmentally friendly materials for sensor fabrication and contribute to addressing industrial waste recycling challenges.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144657828","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"An environmentally relevant solid-state sensor for the trace detection of triclopyr herbicide","authors":"Ayman H. Kamel and Hisham S. M. Abd-Rabboh","doi":"10.1039/D5AY00916B","DOIUrl":"10.1039/D5AY00916B","url":null,"abstract":"<p >A novel solid-contact potentiometric sensor was developed for the selective and trace-level detection of triclopyr (Tcpy), an environmentally persistent pyridine-based herbicide. The sensor comprises a poly(vinyl chloride) (PVC) membrane incorporating tetradecylammonium bromide (TDAB) as the ion-exchanger and <em>o</em>-nitrophenyl octyl ether (<em>o</em>-NPOE) as the plasticizer, supported on a glassy carbon electrode modified with reduced graphene oxide (rGO). The introduction of rGO significantly enhanced the sensor's electron transfer kinetics, signal stability, and interfacial capacitance, enabling a near-Nernstian response of −55.7 mV per decade over a linear concentration range of 3.0 × 10<small>⁻⁶</small> to 1.0 × 10<small>⁻³</small> M, with a detection limit of 7.6 × 10<small>⁻⁷</small> M. The sensor exhibited a fast response time (&lt;5 s), excellent selectivity against structurally related herbicides and common anions, and outstanding potential stability, with a drift as low as 18.3 μV s<small>⁻¹</small>. Its analytical performance was validated through the quantification of triclopyr in spiked environmental water samples and a commercial pesticide formulation (Garlon 3A), with recovery rates ranging from 96% to 102% and results statistically comparable to HPLC measurements. This work demonstrates a cost-effective, reliable, and field-deployable platform for monitoring triclopyr contamination, highlighting the promising role of rGO-based solid-contact ion-selective electrodes in environmental sensing.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 29","pages":" 6018-6025"},"PeriodicalIF":2.7,"publicationDate":"2025-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144635682","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}