Analytical Methods最新文献

{"title":"Surface enhanced Raman scattering (SERS) for the detection of piperine, an active component in herbal formulations.","authors":"G R Advaya, Gaurav Banerjee, Jobin Cyriac","doi":"10.1039/d5ay00991j","DOIUrl":"https://doi.org/10.1039/d5ay00991j","url":null,"abstract":"<p><p>Surface-enhanced Raman scattering (SERS) is a highly sensitive technique that can be used to detect trace amounts of chemicals. We have demonstrated a method using Ag@citrate nanoparticles for detecting piperine. Piperine, the major alkaloid responsible for the pungency and therapeutic properties of black pepper (<i>Piper nigrum</i>) and long pepper (<i>Piper longum</i>), serves as the essential criterion for quality control and authentication. This study demonstrates the efficacy of an economical Raman spectrometer equipped with a portable probe and SERS for the precise identification and quantification of piperine. Substantial signal amplification occurred with Ag@citrate as the substrate, enabling the identification of the characteristic Raman peaks associated with piperine. High sensitivity, repeatability, and specificity were demonstrated by this approach. Inspired by the results, we have done the analysis of two important commercial Ayurvedic medicines, namely <i>Thaleesapathradi choornam</i> and <i>Ashta choornam</i>. Our study demonstrates the potential of SERS as a rapid and effective tool for quality assurance and authenticity verification in the pharmaceutical sector.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145190388","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":"Optimizing the extraction of ursolic acid from loquat leaf using ¹H-qNMR.","authors":"Wen-Ya Lu, Meng-Ting Wang, An-Ya Yang, Yu-Xin Zhang, Bin Zhu, Xiang Wang, Kai Shi, Jiu-Hua Song","doi":"10.1039/d5ay01340b","DOIUrl":"https://doi.org/10.1039/d5ay01340b","url":null,"abstract":"<p><p>Ursolic acid (UA) has a wide range of biological activities and is extracted primarily from natural products. However, conventional quantification methods require derivatization or chromatographic separation, which are tedious and time-consuming. In this study, a rapid and accurate quantitative proton nuclear magnetic resonance (¹H-qNMR) method was established for the direct quantification of UA in loquat leaf extracts. By optimizing the NMR acquisition parameters, ¹H-qNMR achieved a single-sample runtime of 5 min with high accuracy and precision. This method was also applied to optimize UA extraction from loquat leaves, systematically evaluating the effects of temperature, extraction solvent, solid-to-liquid ratio, and extraction time on the purity and yield of UA crude extract. Results indicated that the optimal conditions involved the low-temperature extraction of loquat leaves (sample concentration: 0.03 g mL^-1) with ethanol at 0 °C for 48 h, which afforded an average UA crude purity of 33.68% and an extraction yield of 0.84%, outperforming Soxhlet extraction. This study confirms that ¹H-qNMR enables rapid quality control of UA in loquat and provides a simple, reliable analytical strategy for optimizing extraction processes of bioactive compounds in other complex botanicals.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145190441","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":"Facile detection of illicit wastewater discharge into a water source using a kinetic-based optical fingerprinting strategy.","authors":"Anna V Shik, Ramil M Akhmetov, Gleb K Sugakov, Daria G Filatova, Irina A Doroshenko, Tatyana A Podrugina, Mikhail K Beklemishev","doi":"10.1039/d5ay01066g","DOIUrl":"https://doi.org/10.1039/d5ay01066g","url":null,"abstract":"<p><p>Extensive monitoring of water sources necessitates the development of inexpensive and effective methods for monitoring their pollution. A particularly challenging task is detecting a sudden release of contaminated effluents into a water supply. To solve this issue, we employ a reaction-based fingerprinting technique that is based on conducting an indicator reaction of oxidation of carbocyanine dyes in the presence of a sample. The absorbance and fluorescence intensity are measured periodically using cameras, and the obtained data are processed using machine learning techniques. Monitoring of clean tap or river water was simulated by sampling every few days. Artificial contamination of this water was modeled by adding diluted sewage water (4 different samples). As a result, the contaminated samples were displayed as outliers in the score plots. In both tap and river water, 0.1% vol of wastewater (1000-fold dilution) was detected. The accuracy of discrimination between polluted and unpolluted samples exceeded 90% using linear discriminant analysis (LDA) or softmax regression (SR). Thereby, an unexpected discharge of wastewater into a water source could be rapidly detected with simple instruments. Development of this approach will contribute to improving the accuracy and ease of detection of water source contamination, making environmental monitoring methods more reliable for the benefit of public health.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145197464","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":"WTSynNet: a lightweight cooperative network for multi-species Raman spectral classification.","authors":"Zhishun Huang, Ri-Gui Zhou, Pengju Ren","doi":"10.1039/d5ay01163a","DOIUrl":"https://doi.org/10.1039/d5ay01163a","url":null,"abstract":"<p><p>Animal blood and semen contain diverse biochemical constituents that are of great importance in forensic science, veterinary diagnostics, and species traceability. Raman spectroscopy has emerged as a powerful tool for body fluid identification owing to its non-destructive and rapid acquisition of molecular vibrational fingerprints. However, achieving a balance between discriminative feature extraction and computational efficiency remains a challenge, particularly in imbalanced multiclass scenarios. To address this issue, we propose WTSynNet, a lightweight framework that integrates a one-dimensional wavelet convolution module (WTConv1d) with a star operation mechanism to enable efficient multiscale feature learning. Experiments on animal blood and semen Raman spectral datasets demonstrate that WTSynNet attains over 98% classification accuracy with fewer than 0.3 M parameters, while maintaining extremely low inference latency and memory usage. Moreover, the model achieves strong performance on a cross-domain marine pathogen Raman dataset, underscoring its robustness and adaptability. These results indicate that WTSynNet is a compact yet powerful model with strong generalization capability and holds broad potential for future applications in rapid on-site Raman spectral analysis.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145197527","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 study on selective profiling of cardiovascular and cerebrovascular disease-associated proteins using two statin-based magnetic separation materials.","authors":"Yanfeng Zheng, Yini Pan, Zhenxin Wang, Zhichao Yan, Lingyi Zhang, Weibing Zhang","doi":"10.1039/d5ay01174d","DOIUrl":"https://doi.org/10.1039/d5ay01174d","url":null,"abstract":"<p><p>This study established a drug-associated protein screening strategy leveraging the principle of specific protein-drug interactions. Two first-line lipid-lowering drugs, atorvastatin (AN) and rosuvastatin (RSV), were covalently immobilized onto nanoparticle surfaces to fabricate novel magnetic separation materials, Fe₃O₄@AN and Fe₃O₄@RSV. Initial validation of the strategy was performed using fetal bovine serum (FBS) as a model sample, with alterations in protein amino acid sequence coverage serving as the evaluation parameter. Fe₃O₄@AN specifically adsorbed four proteins from FBS, all of which were implicated in cardiovascular diseases (CVDs). Similarly, Fe₃O₄@RSV enriched five CVD-associated proteins from FBS. Three proteins (Q3T052, P1276, and Q58D62) were co-enriched by the two materials. Subsequently, the developed strategy was applied to clinical serum samples from CVD patients and healthy controls to screen disease-relevant proteins <i>via</i> label-free quantitative proteomics. Comparative analysis revealed that Fe₃O₄@AN and Fe₃O₄@RSV selectively enriched 23 and 37 differentially expressed proteins (DEPs) from sera of CVD patients and healthy controls, respectively. Gene Ontology (GO) and pathway enrichment analyses indicated distinct functional pathways for proteins captured by each material, and both sets were found to be significantly associated with CVD-related biological processes and cellular components. Notably, six overlapping DEPs were co-identified by the two materials, all demonstrating critical functions in CVD pathogenesis. Among these, two proteins (P02042 and P14174) were exclusively detected in patient sera, while Q14624 was detectable in CVD patient serum, healthy human serum, and FBS but significantly upregulated in CVD patient serum. Collectively, this protein-drug interaction-based screening strategy exhibits broad applicability and establishes a novel paradigm for rational drug design and development.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145184307","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 smartphone-based colorimetric chemosensor for on-site detection of indium ions in environmental water samples: solution and solid-state analysis.","authors":"Savikriti Saini, Selva Kumar Ramasamy, Vetriarasu Venkatesan","doi":"10.1039/d5ay01214g","DOIUrl":"https://doi.org/10.1039/d5ay01214g","url":null,"abstract":"<p><p>A novel diaminomaleonitrile-based colorimetric probe, 2-amino-3-[(8-hydroxy-2-quinolinyl)methylene]amino]-2-butenedinitrile (HQ-DAMN), was successfully synthesized and extensively characterized using a range of spectroscopic techniques. The sensing ability of HQ-DAMN towards multiple cations was investigated using colorimetric analysis, paper strips, an RGB model, alginate beads, and a UV-Vis spectrophotometer method in ACN: H₂O (4 : 6, v/v, pH 6.5). Upon interaction with the In³⁺ ion, the colorless solution of HQ-DAMN immediately transforms into orange, while no visible color change was observed with other metal ions. UV-Vis spectrophotometric studies revealed that HQ-DAMN exhibits a strong absorption peak at 374 nm and a weak absorption peak at 266 nm, attributed to intramolecular charge transfer (ICT) and ligand-to-ligand charge transfer (LLCT), respectively. Upon binding with the In³⁺ ion, new peaks emerge at 472 nm, indicative of ligand-to-metal charge transfer (LMCT). The HQ-DAMN-In³⁺ complex exhibited a 2 : 1 binding stoichiometry, with a binding constant of 7.70 × 10³ M^-2, as determined using Job's plot and Benesi-Hildebrand (B-H) plot analysis. HQ-DAMN was found to be stable in a pH range of 4.0-7.0, retaining its high selectivity in the presence of competing ions. Moreover, it achieved excellent sensitivity, with detection limits as low as 66.7 nM using spectrophotometric methods and 0.68 μM with the RGB model. The interaction between HQ-DAMN and In³⁺ ions was thoroughly investigated using ¹H NMR spectra, ESI mass spectrometry, and FT-IR spectroscopy, supported by theoretical computational studies. These findings affirm the potential of HQ-DAMN as a colorimetric and smartphone RGB sensor for In³⁺ ion detection.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145184288","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":"Application of azacyclobutane modified perylene imide fluorescent probes targeting lipid droplets in the diagnosis of metabolic dysfunction-associated fatty liver.","authors":"Lixia Zhang, Tingting Hao, Yongqing Wang, Lin Cai, Rui Huang, Hongmei Liu","doi":"10.1039/d5ay01145k","DOIUrl":"https://doi.org/10.1039/d5ay01145k","url":null,"abstract":"<p><p>Fatty liver can be divided into metabolic dysfunction-associated fatty liver disease, alcoholic fatty liver and special type fatty liver. Among them, MAFLD is generally ignored due to its early clinical symptoms, which can lead to malignant diseases such as cirrhosis and liver cancer in the long run. Therefore, early diagnosis and treatment can effectively prevent malignant lesions, so as to ensure good health and improve the quality of life. As a specific index of MAFLD, the dynamic change in lipid droplets can also reflect the change in the disease course. Therefore, we conducted relevant biological experiments on the newly synthesized azacyclic butane perylene imide a fluorescent probe (PDIs-560) targeting lipid droplets. The results show that it not only has excellent targeting of lipid droplets <i>in vivo</i> but also can detect lipid droplets quickly and sensitively in the MAFLD mouse model. This method of <i>in situ</i>, real-time and non-destructive detection of lipid droplets by the PDIs-560 fluorescent probe is expected to provide a new way for early clinical diagnosis and monitoring of MAFLD.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145184242","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":"A dual ligand Eu-MOF with high stability and quantum yield for the detection of trace Fe³⁺, CrO₄^2- and Cr₂O₇^2- in aqueous environments.","authors":"Nanhai Zhang, Deyan Liu, Rui Zhang, Qinghe Song, Guangjun He, Shixing Wang, Libo Zhang","doi":"10.1039/d5ay01329a","DOIUrl":"https://doi.org/10.1039/d5ay01329a","url":null,"abstract":"<p><p>The design and preparation of fluorescent sensors for detecting toxic ions in aqueous environments are of paramount importance. In this study, a europium metal-organic framework (Eu-MOF), constructed from Eu³⁺, the rigid 2,2'-biphenyldicarboxylic acid (2,2'-H₂bpdc) ligand, and the auxiliary 1,10-phenanthroline (Phen) ligand, was synthesized through hydrothermal synthesis. The synthesized Eu-MOF demonstrated remarkable water stability, pH stability, thermal stability, and photostability. It showed a high quantum yield of 42.6%, along with an average fluorescence lifetime of 0.9002 ms, which could enhance its sensitivity when employed as a fluorescent probe. The Eu-MOF could function as a fluorescent probe to quantitatively detect trace amounts of Fe³⁺, CrO₄^2- and Cr₂O₇^2-<i>via</i> fluorescence quenching. Their detection sensitivities are 1.527 × 10⁴ M^-1, 1.378 × 10⁴ M^-1 and 1.463 × 10⁴ M^-1 respectively, with detection limits as low as 0.28 μM, 0.19 μM and 0.09 μM. Additionally, the Eu-MOF sensor exhibited excellent selectivity, anti-interference ability, repeatability (after undergoing five cycles) and practical feasibility. Furthermore, a detailed investigation of its fluorescence properties and sensing mechanisms was carried out. Based on density functional theory calculations, two energy transfer pathways in the process of Eu³⁺ ion luminescence sensitized by the double ligands 2,2'-H₂bpdc and Phen were identified. The fluorescence sensing mechanism of the Eu-MOF for detecting Fe³⁺, CrO₄^2- and Cr₂O₇^2- involved photoinduced electron transfer from the antenna ligand to the organic molecules and competitive absorption of excitation energy. Owing to its high stability and sensitivity, the Eu-MOF holds great potential for practical applications as a sensor for Fe³⁺, CrO₄^2- and Cr₂O₇^2- in aqueous environments.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145184264","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":"Rotating gold microwire electrode for the voltammetric detection of mercury and arsenic in shellfish.","authors":"Wesley J McCormick, Eveline Düker, Matthew McCole, Christopher McEleney, Denis McCrudden","doi":"10.1039/d5ay01018g","DOIUrl":"https://doi.org/10.1039/d5ay01018g","url":null,"abstract":"<p><p>Monitoring mercury (Hg) and arsenic (As) in bivalve shellfish is crucial for ensuring food safety and protecting human health, given the bioaccumulation potential of these toxic contaminants. This study introduces a novel, low-cost, and highly sensitive electrochemical method for the determination of Hg and As in bivalve molluscs, leveraging a unique assembly that incorporates a gold micro-electrode. The electrode's design is characterised by its increased surface area resulting from the spherical geometry, enhancing sensitivity for trace metal detection. Further refinement is achieved through the integration of a conductive coupler, facilitating the electrode's rotation to augment analyte mass transport to the electrode surface, thereby improving the detection limits and overall analysis efficiency. The simplicity of the sensor assembly combined with its capacity for on-site and <i>in situ</i> application, sets a new benchmark for practicality in environmental monitoring tools. After pretreatment and conditioning of the substrate its ability to detect trace levels of As and Hg in certified reference materials and in real shellfish samples after microwave digestion was investigated. The repeatability, linearity, accuracy, and detection limit of the procedure were evaluated. For mercury and arsenic, a short 90 second deposition time resulted in detection limits of 0.3 μg L^-1 and 0.21 μg L^-1 and a linearity of 0.5 to 100 μg L^-1 and 1.0 to 100 μg L^-1, respectively. Close agreement with stated values for a certified reference material verified the accuracy and reliability of the analysis.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145184247","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":"Effects of microscans on the results of orbitrap mass spectrometry analysis of natural organic matter.","authors":"Sophia M Byvsheva, Mikhail A Proskurnin, Dmitry S Volkov","doi":"10.1039/d5ay01313e","DOIUrl":"https://doi.org/10.1039/d5ay01313e","url":null,"abstract":"<p><p>This study experimentally confirms that averaging individual spectral transients (microscans) is not equivalent to averaging scans in the enhanced FT algorithm of data acquisition within the orbitrap performance. The effect of microscans on the absolute noise level is studied; signal-to-noise ratio (SNR) and results of qualitative molecular analysis of natural organic matter (NOM) were obtained. Our studies have shown significant differences in the structure of obtained spectra and especially in the intensity and appearance of noise signals. Increasing the number of microscans leads to an increase in SNR, which is especially important for systems with a large content of low-intensity analytical peaks like NOM. The influence is significant and must be considered both during in-laboratory measurements for various samples and when comparing results across different laboratories.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.6,"publicationDate":"2025-09-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145147292","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}