Analytical Methods最新文献

{"title":"FeCu3-LDH/MoS2 superlattice-modified carbon paper as an integrated sensor for the sensitive detection of nitrofurantoin in various samples†","authors":"Xueting Wang, Yuehua Li, Boran Tong, Xingwen Wang, Wei Meng, Jing Zhang and Chao Han","doi":"10.1039/D5AY00463B","DOIUrl":"10.1039/D5AY00463B","url":null,"abstract":"<p >Nitrofurantoin (NFT) is a broad-spectrum antibiotic used for the treatment of humans, poultry and livestock. Improper use and discharge of NFT can cause serious harm to human health and the environment. Electrochemical analysis has been widely employed in antibiotic detection because of its advantages of simple operation, high sensitivity and rapid response. However, few studies have reported the detection of NFT using this method owing to the limited availability of electrode materials. Layered double hydroxides (LDHs) have attracted widespread attention because of their unique structure and chemical properties as well as the advantages of homogeneous dispersion of laminate elements and adjustable chemical composition. However, their application in NFT detection has rarely been reported due to the inherent defects of weak conductivity and poor stability. To better use LDHs and overcome their shortcomings, a series of superlattice FeCu<small>₃</small>-LDH/MoS<small>₂</small> materials were successfully designed using stripping and self-assembly strategies. FeCu<small>₃</small>-LDH/MoS<small>₂</small> modified carbon paper (CP) was used as an integrated sensor for NFT detection. Benefiting from the structural advantages of the superlattice material and dual-synergistic catalysis between the LDH and MoS<small>₂</small>, FeCu<small>₃</small>-LDH/MoS<small>₂</small>/CP (1 : 1) exhibited highly sensitive NFT detection, with a low detection limit. FeCu<small>₃</small>-LDH/MoS<small>₂</small>/CP (1 : 1) could also be successfully applied for NFT determination in real samples, such as human serum, lake water and commercialized drugs, with satisfactory recovery. This work not only provides an effective electrochemical detection method for NFT determination, but also broadens the application of LDHs in the electrochemical field and lays a foundation for the controllable preparation of electrochemical sensors based on superlattice materials.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 28","pages":" 5886-5896"},"PeriodicalIF":2.7,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144558532","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 systematic review of separation/preconcentration and detection techniques for speciation analysis of arsenic and selenium in water","authors":"Yanping Li, Cuicui Wang, Jianchao Zhao, Xiaoqi Liu, Mingyuan Ma, Ai Gao and Kangrui Sun","doi":"10.1039/D5AY00626K","DOIUrl":"10.1039/D5AY00626K","url":null,"abstract":"<p >The speciation of arsenic and selenium in aquatic environments has garnered significant research attention owing to the critical relationship between elemental speciation and both toxicity profiles and bioavailability mechanisms. Over the past two decades, substantial progress has been achieved in developing advanced analytical methodologies for speciation analysis, particularly addressing the challenges posed by arsenic's pronounced toxicity and selenium's dual biological roles. This review systematically examines the separation/preconcentration techniques and detection strategies employed in various aqueous matrices, including riverine systems, lacustrine environments, marine waters, and surface water bodies. A comprehensive evaluation of pretreatment technologies reveals that the matrix complexity and ultra-trace concentration requirements continue to drive methodological innovations, with particular emphasis on solid-phase extraction and chromatographic separation techniques. Analytical advancements are critically assessed through comparative analysis of spectroscopic detection methods (<em>e.g.</em>, ICP-MS, AAS, AFS) coupled with separation modalities (<em>e.g.</em>, HPLC, IC, MSPE). Critical validation parameters—including detection limits, recovery rates, precision, and enrichment factors—were systematically summarized alongside methodological characteristics such as typical separation media, key devices employed. Studies have shown that although some new pretreatment and detection technologies have emerged, hyphenated techniques still remain the mainstream in speciation analysis research. The review concludes with evidence-based recommendations for method selection guided by sample matrix characteristics and target speciation requirements while highlighting the imperative for continued innovation in achieving species-specific detection at environmentally relevant concentrations.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 28","pages":" 5807-5830"},"PeriodicalIF":2.7,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144558517","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 fluorescein based dual optical sensor for highly selective and sensitive fluoride detection in 100% water medium†","authors":"Bikash Chandra Mushahary, Debajit Bora, Chayanika Goswami, Mayur Jyoti Bhuyan, Sudhangshu Priya Bharati, Rituraj Das and Sanjeev Pran Mahanta","doi":"10.1039/D4AY02287D","DOIUrl":"10.1039/D4AY02287D","url":null,"abstract":"<p >A highly selective dual optical sensor for fluoride detection in 100% aqueous medium is reported, utilizing an Al<small>³⁺</small>-complex of fluorescein. The sensor exhibits distinct colorimetric and fluorometric responses, achieving detection limits of 0.7 ppm (UV-Vis) and 40 ppb (fluorescence). This method, validated on water samples and cellulose paper strips, offers a practical, low-cost approach for routine fluoride monitoring.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 29","pages":" 5997-6001"},"PeriodicalIF":2.7,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144641265","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":"Exposing active sites in zeolites with fluoropyridines as NMR probe molecules.","authors":"Joseph Hurd, Yujie Ma, Paolo Cerreia Vioglio, Run Zou, Dinu Iuga, Sihai Yang, Xiaolei Fan, Daniel Lee","doi":"10.1039/d5ay00507h","DOIUrl":"10.1039/d5ay00507h","url":null,"abstract":"<p><p>Active sites in zeolites are crucial for catalysis, but their identification remains challenging due to structural complexity. Solid-state NMR, a key tool for studying zeolites, can struggle with directly detecting acidic properties due to the quadrupolar nature of ubiquitous metal dopants. Here, we use fluorinated pyridine as a probe to identify active sites in HY and HZSM-5, two important solid acid catalysts. ¹⁹F NMR effectively detects binding environments, while ¹⁹F-²⁷Al polarization transfer reveals elusive penta-coordinated Al^V Brønsted acid sites and shows that the dominant active sites are distorted framework-associated Al^IV and Al^V sites with large quadrupolar coupling constants, shedding light on catalytic properties. Low-temperature (100 K) NMR proves essential for capturing these interactions. This work enhances the understanding of zeolite active sites and highlights the broad applicability of fluorinated probe molecules for surface characterization, offering a cost-effective, highly sensitive approach for catalytic studies.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12227064/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144558531","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Facile and highly sensitive nitrate ion detection via an electrochemical sensor based on a poly 1,8-diaminonaphthalene and copper oxide particle film†","authors":"Saad Benhaiba, Anas El Attar, Ouissal Salhi, Badr Bouljoihel, Charafeddine Jama, Soad Youssefi, Amine Ezzahi and Mama El Rhazi","doi":"10.1039/D5AY00655D","DOIUrl":"10.1039/D5AY00655D","url":null,"abstract":"<p >Excessive nitrate accumulation in soil and water has become a critical environmental concern, threatening ecosystems and public health. This drives the need for designing new electrochemical nitrate sensors based on novel electroactive materials. In this work, we synthesized a hybrid film material composed of poly 1,8-diaminonaphthalene and copper oxide particles electrodeposited on the surface of a carbon paste electrode (Cu<small>₂</small>O–CuO/poly 1,8-DAN/CPE). The electrodeposition of the polymer was conducted in galvanostatic mode at a positive current, followed by the electrodeposition of copper in potentiostatic mode at a negative potential. The polymeric film obtained through this facile electropolymerization method showed a uniform dispersion of copper particles and could improve the mechanical stability of the fabricated sensors, thereby leading to a low detection limit of nitrate ions. The Cu<small>₂</small>O–CuO/poly 1,8-DAN/CPE was prepared in just 3 min in both the galvanostatic and potentiostatic mode. The developed sensor exhibited a good electrochemical performance for nitrate ions, with a linear range from 2 to 200 μM, strong stability, high reproducibility, and a low detection limit of 0.5 μM. This work revealed that the deposition of polymer can be applied as a promising material in new applications, such as water denitrification.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 28","pages":" 5868-5885"},"PeriodicalIF":2.7,"publicationDate":"2025-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144551459","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":"Characterization of non-volatile compounds, volatile compounds, and inorganic elements in different growth stages of Scutellariae Radix†","authors":"Shuang Liu, Heping Jiao, Chuanzhi Kang, Zhenhua Wang, Xiao Wang and Hongjing Dong","doi":"10.1039/D5AY00762C","DOIUrl":"10.1039/D5AY00762C","url":null,"abstract":"<p >Scutellariae Radix (SR) is a traditional Chinese medicine recognized for its potential to treat various disease conditions. SR is primarily investigated in clinical settings in two forms, namely Ziqin and Kuqin, each exhibiting distinct effects. However, few studies have systematically examined the differences in compounds and inorganic element content between the two forms. Therefore, this study aims to analyze the non-volatile and volatile compounds using UPLC-HRMS and GC-IMS, as well as the inorganic elements using ICP-MS. The results suggested significant differences in the content of non-volatile compounds, particularly flavonoids, between Ziqin and Kuqin. Kuqin demonstrated a higher content of flavonoids and volatile compounds compared to Ziqin. Moreover, the inorganic elements (particularly Cu and Al) might influence the content of flavonoid compounds by regulating their biosynthesis. This study identifies potential chemical markers that may contribute to the distinct therapeutic profiles, and these findings provide a basis for future pharmacological investigations.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 29","pages":" 6009-6017"},"PeriodicalIF":2.7,"publicationDate":"2025-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144625020","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":"Upconversion fluorescence immunochromatographic assay for highly sensitive and rapid detection of ovarian function indicators: follicle-stimulating hormone and anti-Müllerian hormone†","authors":"Jianfeng Yao, Ming Li, Rongfu Huang, Yanting Wang, Liang Song, Liying Chen and Zhenzhu Zheng","doi":"10.1039/D5AY00500K","DOIUrl":"10.1039/D5AY00500K","url":null,"abstract":"<p >The assessment of ovarian function is crucial for female reproductive health, assisted reproduction, and the early detection of gynecological diseases. Follicle-stimulating hormone (FSH) and anti-Müllerian hormone (AMH), two key markers of ovarian function, are essential for accurate evaluations that guide clinical decision-making. However, conventional detection techniques, such as ELISA, face limitations including low sensitivity, poor specificity, and prolonged detection times. To overcome these challenges, we developed an upconversion fluorescence immunochromatographic assay for highly sensitive and rapid detection of FSH and AMH. This method harnesses the unique properties of upconversion luminescence to minimize interference from background fluorescence, enabling swift and precise detection. The assay achieves detection within 15 min, with established limits of 0.097 ng mL<small>⁻¹</small> for FSH and 0.018 ng mL<small>⁻¹</small> for AMH. Moreover, it demonstrated remarkable performance in serum sample testing, yielding a recovery range of 92.56–97.80%, with coefficients of variation below 10%. Additionally, the assay offers qualitative visual analysis using upconversion green fluorescence, meeting the needs of both clinicians and home-based patient assessments. In summary, the method we developed provides robust technical support for clinical ovarian function assessments.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 29","pages":" 6026-6033"},"PeriodicalIF":2.7,"publicationDate":"2025-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144635684","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":"Selenium and organic- and inorganic-Hg in stir-fried mushrooms†","authors":"Jerzy Falandysz, Yuanzhong Wang, Małgorzata Rutkowska, Anetta Hanć and Alwyn R. Fernandes","doi":"10.1039/D5AY00794A","DOIUrl":"10.1039/D5AY00794A","url":null,"abstract":"<p >Selenium (Se) and co-occurring total and organic mercury (THg and o-Hg) were investigated in wild edible mushroom species collected from Central Yunnan, Southwestern China. The regional terrain is known for being Se-deficient and consequential diseases such as Keshan and Kashin–Beck are endemic. “Pseudo-porcini” species, <em>Boletus bainiugan</em> and <em>Butyriboletus roseoflavus</em>, were Se-rich (means of 28 and 13 mg kg<small>⁻¹</small> dry weight), while six other species contained tenfold lower concentrations. The two bolete species contained 4.1 and 2.8 mg kg<small>⁻¹</small> dw of THg and 0.047 and 0.038 mg kg<small>⁻¹</small> dw of o-Hg, respectively, with means of 0.22 and 0.01 mg kg<small>⁻¹</small> dw in other species. Stir-frying enhanced analyte concentrations, favoring Se relative to Hg, in most species, particularly boletes. Health risk-benefit assessments of the stir-fried mushrooms using both the Se : Hg molar quotient and the Se health benefit value (HBVSe) showed strongly positive values for boletes and were favorable for other species except for <em>Scleroderma yunnanense</em>.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 27","pages":" 5788-5794"},"PeriodicalIF":2.7,"publicationDate":"2025-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144551460","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":"Recent advances in small-molecule fluorescent probes bearing a triaminoguanidinium unit and their sensing, bio-imaging and multifunctional applications","authors":"Balamurugan Tharmalingam","doi":"10.1039/D5AY00771B","DOIUrl":"10.1039/D5AY00771B","url":null,"abstract":"<p >Since their discovery, triaminoguanidinium-salicylidene-based Schiff bases have emerged as a significant class of compounds known for their solvent-dependent fluorescence emission, which varies depending on the substituents in their aromatic frameworks. These compounds are easy to synthesize, stable, cost-effective, and highly suitable for diverse applications, including chemosensing, biological studies, and multifunctional uses. This comprehensive review summarizes recent advancements in AIE-active triaminoguanidinium-salicylidene-based threefold symmetric Schiff molecules, particularly their role as chemosensors for detecting various analytes. It explores different chemosensing strategies for identifying metal ions (Zn<small>²⁺</small>, Cd<small>²⁺</small>, Cu<small>²⁺</small>, Fe<small>³⁺</small>, and Co<small>²⁺</small>) and anions (EDTA, I<small>⁻</small> PPi<small>⁻</small>, and S<small>²⁻</small>), focusing on the progress of triaminoguanidinium-salicylidene-based threefold symmetric Schiff bases over the past five years, particularly their systems for supramolecular host–guest interactions, AIEgen-ESIPT activity, COFs, bioimaging, <em>etc</em>. We hope this review provides a comprehensive overview of the current research landscape and encourages further exploration of novel triaminoguanidinium-salicylidene-based threefold symmetric Schiff base compounds with expanded applications.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 27","pages":" 5579-5604"},"PeriodicalIF":2.7,"publicationDate":"2025-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144537484","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 an assay method for tofersen using IPRP-LC-HRMS with an extracting ion chromatogram processing approach†","authors":"Anuradha A. Hargude, Vijay S. Bhalekar and Ravi P. Shah","doi":"10.1039/D5AY00666J","DOIUrl":"10.1039/D5AY00666J","url":null,"abstract":"<p >The quality control of oligonucleotides using separation analytical methods is complicated owing to co-elution of structurally similar impurities and active oligonucleotides. Thus, the inadequate separation of impurities from the active pharmaceutical ingredients restricts the applicability of these assay methods. This limitation also hinders achieving compliance with regulatory standards. Accordingly, this research was focused on the development of an assay methodology for tofersen (TSN) to enable accurate quantification despite the presence of co-eluting impurities. An analytical assay method for the determination of TSN was proposed based on ion-pair reverse-phase liquid chromatography coupled with high-resolution mass spectrometry using an extracted ion chromatography processing approach. Nusinersen (NSN) was utilized as the internal standard to mitigate variations in signal intensity of the mass spectrometer. The developed method was validated according to the ICH Q2(R2) and USP regulatory frameworks. The method demonstrated linear response and specificity within the concentration range of 3–10 μg mL<small>⁻¹</small>. The recovery from the formulation matrix, which was determined using the standard addition method with triplicate measurements at three concentration levels, was found to be within the range of 80–120%. Furthermore, the method exhibited precision and robustness for critical liquid chromatography parameters, such as flow rate and injection volume, and mass spectrometer parameters, including drying/desolvation temperature and gas flow.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 27","pages":" 5636-5643"},"PeriodicalIF":2.7,"publicationDate":"2025-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144537418","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}