Analyst最新文献

{"title":"Development of highly sensitive, highly selective and high-throughput method for determination of total ascorbic acid","authors":"Takeru Koga, Aina Yoshida, Mayuko Tomisawa, Mitsuhiro Nakamura, Akihiro Tai","doi":"10.1039/d5an00319a","DOIUrl":"https://doi.org/10.1039/d5an00319a","url":null,"abstract":"A highly sensitive, highly selective, and high-throughput method for determination of intracellular total ascorbic acid (AA) was developed by measuring the fluorescence intensity of 1,2-diamino-4,5-methylenedioxibenzene (MDB)-labeled AA. First, the reaction buffer, temperature, pH, and time were investigated to establish optimal reaction conditions, and it was found that AA was detected with high sensitivity by reacting oxidized AA and MDB in 100 mM citrate buffer (pH 5.0) for 10 min at room temperature. Next, a scale-up synthesis was performed to determine the chemical structure of the MDB-labeled AA, and its excitation and emission wavelengths were optimized to 375 and 450 nm, respectively. HPLC analysis revealed that MDB reacts with AA with high selectivity under the established conditions. It was also found that AA could be determined under optimal reaction conditions, regardless of the presence or absence of cellular components. In conclusion, the established method for determination of AA with MDB can quantify AA in the range of 25 nM to 20 µM in a microplate with a detection limit of 10 nM. Furthermore, the method was confirmed to be able to quantify intracellular AA in a cell line by comparison with a standard HPLC method. This method is applicable to highly sensitive, highly selective, and high-throughput analysis and could be applied to the determination of AA in various cells used in the evaluation of AA activity.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"152 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144145676","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":"Measuring the hydrodynamic radii of peptides and proteins with an unmodified LC-ESI-MS instrument operating in a Taylor dispersion regime","authors":"Jonathan Eisert, Edvaldo Vasconcelos Soares Maciel, Henrik Jensen, Frederik Lermyte","doi":"10.1039/d5an00344j","DOIUrl":"https://doi.org/10.1039/d5an00344j","url":null,"abstract":"Native ion mobility – mass spectrometry has been well established in recent years as a structural biology method. However, it is still useful to combine gas-phase techniques with complementary solution-phase measurements, for example hydrodynamic radius (<em>R</em><small>_h</small>) determination. A common method to measure protein <em>R</em><small>_h</small> is the use of Taylor dispersion analysis (TDA), which relies on measuring the longitudinal dispersion of an analyte in a laminar flow within a capillary. This type of analysis most often relies on spectroscopic (<em>e.g.</em>, fluorescence-based) detection, although a few studies have reported the use of custom-built or modified fluidics systems coupled with MS-based detection. Here, we have repurposed a standard, unmodified LC-MS system, operated without a column, to measure hydrodynamic radii of peptides and proteins, including noncovalent complexes, ranging from 300 Da to 133 kDa. The <em>R</em><small>_h</small> values we measured showed excellent correlation with gas-phase collision cross-sections as well as <em>R</em><small>_h</small> values measured with a conventional TDA instrument with fluorescence-based detection. Notably, due to the mass-selective readout of our method, which is based on analysis of extracted ion chromatograms, we were able to perform multiplexed <em>R</em><small>_h</small> measurements of several proteins in a single experiment, and also measured apparent <em>R</em><small>_h</small> values for different oligomeric states of BSA and concanavalin A. Consistent with prior literature, the latter data suggested that concanavalin A primarily exists as a dimer and tetramer in solution, with monomer signals being largely due to dissociation during electrospray ionisation. We have named our method <strong>Hyd</strong>rodynamic <strong>Ra</strong>dii from an <strong>U</strong>nmodified <strong>Li</strong>quid <strong>C</strong>hromatography-<strong>M</strong>ass <strong>S</strong>pectrometer (HYDRAULIC-MS).","PeriodicalId":63,"journal":{"name":"Analyst","volume":"213 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144145675","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":"Programmable wide-range pH gradients for NMR titrations: application to antibody-drug conjugate linker group modifications","authors":"Matthew Wallace, James M. Sharpe, Krzysztof Baj, Michael Ngwube, Jenny Thirlway, Patrick L. Kerigan Higgs, G. Richard Stephenson, Jonathan Iggo, Thomas Edward Storr, Chris J Richards","doi":"10.1039/d5an00406c","DOIUrl":"https://doi.org/10.1039/d5an00406c","url":null,"abstract":"We generate pH gradients spanning more than six units in standard NMR tubes and determine all the p<em>K</em><small>_a</small> values of polyprotic compounds in single 20 minute chemical shift imaging (CSI) NMR experiments. The modest demands of our method in terms of sample quantity and preparation time allow it be performed as part of the routine characterisation and optimisation of organic molecules during synthesis campaigns. As proof of concept, we measure the p<em>K</em><small>_a</small> values of a family of vinylpyridines employed as antibody drug conjugate linkers. Our analysis reveals a strong correlation between the experimental aqueous p<em>K</em><small>_a</small> and the rate of conjugate addition of thiol nucleophiles to the vinyl group, representing a powerful predictive method.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"81 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144136697","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":"Small molecular N-heteroaromatics-based optical sensing of noxious Hg2+ ion: A comprehensive insight into recent advancements, existing challenges, and future perspective","authors":"Kingshuk Debsharma, Sunanda Dey, Basudeb Dutta, Swapan Dey","doi":"10.1039/d5an00538h","DOIUrl":"https://doi.org/10.1039/d5an00538h","url":null,"abstract":"The surrounding ecology and extant mammalian health recognize that the Hg2+ ions are very toxic and can damage the ecosystem even at a trace concentration level. Mercury exposure creates severe adverse effects on human health related to the respiratory system, central nervous system (CNS), skin damage, kidney failure, and various mental disorders. Therefore, detection and estimation of Hg2+ ions by alternative up-to-date techniques are more crucial than traditional methods, which require expensive and skilled personnel. Due to their high sensitivity and selectivity, optical sensors draw much attention for the sensitive and selective detection of various toxic environmental species. Recently, small molecular probes with N-heterocyclic fluorophoric receptors have successfully been utilized in different sensing arenas due to their cost-effective synthesis and commendable photophysical activities. For the last fifteen years, numerous research groups have reported N-heterocyclic-based receptors for Hg2+ ion sensing in solution and solid-state with a selective sensitivity, reversibility, and low limit of detection, accompanying several real-world applications. This review article aims to provide current progress and future viewpoints in N-heteroaromatic-based colorimetric and/or fluorogenic Hg2+ ion sensors with wide real-time applications.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"38 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144122425","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":"The effects of different plasticisers on the electrochemical performance of bespoke conductive additive manufacturing filaments using recycled PLA","authors":"Robert D. Crapnell, Iana V. S. Arantes, Elena Bernalte, Evelyn Sigley, Graham C. Smith, Thiago R. L. C. Paixão, Craig E. Banks","doi":"10.1039/d4an00969j","DOIUrl":"https://doi.org/10.1039/d4an00969j","url":null,"abstract":"In this work, we report the production, physicochemical, electrochemical, and electroanalytical characterisation of 10 different bespoke additive manufacturing filaments that utilise different chemicals as plasticisers. The inclusion of a plasticiser within a recycled poly(lactic acid) based additive manufacturing filament produced through thermal mixing is required when incorporating high loadings of conductive fillers. All 10 chemicals used in this work acted as suitable plasticisers for producing conductive filaments, allowing the incorporation of 25 wt% carbon black with 65 wt% recycled poly(lactic acid) whilst ensuring excellent low-temperature flexibility and printability. The surfaces of the additive manufactured electrodes were characterised before and after electrochemical activation, revealing a significant increase in the amount of graphitic carbon present after activation in all cases. Through electrochemical characterisation against [Ru(NH<small>₃</small>)<small>₆</small>]<small>³⁺</small> and [Fe(CN)<small>₆</small>]<small>⁴⁻</small>, as well as through the electroanalytical detection of dopamine, castor oil, tris(2-ethylhexyl) trimellitate, and poly(ethylene glycol) were identified as the best overall performing plasticisers for the production of additively manufactured electrodes.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"8 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144113442","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":"Feasibility of non-invasive measurement of cardiac biomarkers using mid-infrared spectroscopy: finite element analysis and experimental validation","authors":"Qingchao Zhang, Yuxuan Xing, Kaizheng Wang, Qiushuo Wu, Yang Zheng, Jian Wu, Xian Huang","doi":"10.1039/d5an00335k","DOIUrl":"https://doi.org/10.1039/d5an00335k","url":null,"abstract":"Attenuated total reflectance mid-infrared (ATR-MIR) spectroscopy provides a quick and efficient way to identify protein-specific absorption spectra, making it a promising technique for the non-invasive detection of cardiac biomarkers that are thought to be direct indicators of major cardiovascular events. However, there are still questions about the effectiveness of ATR-MIR in identifying various critical cardiac biomarkers and the detection depth of evanescent waves. This study employs finite element simulations to examine the optical path of attenuated total reflectance (ATR) and the detection depth of evanescent waves. To simulate a subcutaneous tissue environment, a polydimethylsiloxane (PDMS) reagent bath, a high-density melamine sponge, and a poly(ethylene terephthalate) (PET) film are used to assess the ability of MIR spectroscopy to detect cardiac biomarkers at different depths. The findings reveal that the absorption spectra of cardiac troponin I (cTnI), N-terminal pro-B-type natriuretic peptide (NT-proBNP), and C-reactive protein (CRP) show distinct characteristic peaks in the amide I and amide II bands with high specificity. At a depth of about 15 μm, the peak amplitude shows a strong correlation with the biomarker concentration. Even at a depth of 80 μm, the absorption spectrum of cTnI still displays significant characteristic peaks, confirming its ability to detect subcutaneous superficial cardiac biomarkers. This research underscores the considerable potential of ATR-MIR spectroscopy for the non-invasive detection of subcutaneous cardiac biomarkers, which could aid in the development of wearable devices for monitoring cardiovascular health, ultimately contributing to the prevention, diagnosis, and treatment of cardiovascular diseases.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"78 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144113443","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":"Expression of concern: Amplified plasmonic detection of DNA hybridization using doxorubicin-capped gold particles","authors":"Jolanda Spadavecchia, Ramesh Perumal, Alexandre Barras, Joel Lyskawa, Patrice Woisel, William Laure, Claire-Marie Pradier, Rabah Boukherroub, Sabine Szunerits","doi":"10.1039/d5an90035b","DOIUrl":"https://doi.org/10.1039/d5an90035b","url":null,"abstract":"Expression of concern for ‘Amplified plasmonic detection of DNA hybridization using doxorubicin-capped gold particles’ by Jolanda Spadavecchia <em>et al.</em>, <em>Analyst</em>, 2014, <strong>139</strong>, 157–164, https://doi.org/10.1039/C3AN01794J.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"11 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144096999","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":"Long-term device stability for Raman spectroscopy","authors":"Shuxia Guo, Anuradha Ramoji, Aikaterini Pistiki, Yilmaz Hulya, Uwe Glase, David L Vasquez-Pinzon, Iwan W. Schie, Ute Neugebauer, Anja Silge, Juergen Popp, Thomas Bocklitz","doi":"10.1039/d5an00255a","DOIUrl":"https://doi.org/10.1039/d5an00255a","url":null,"abstract":"Long-term stability of Raman setups is one of the critical criteria for using Raman spectroscopy in real-world applications. Substantial differences from long-term drifts of a device can largely reduce the reliability of the technology and lead to serious consequences in scenarios such as disease diagnostics. A systematic investigation of long-term device stability is urgently needed to understand the device-related variations and to help improve the situation. In this study, 13 substances were measured as quality control references weekly for 10 months on a Raman device as quality control references to investigate instrumental stability over time. The 13 substances were selected to be stable and to cover a wide range of standards, solvents, lipids, and carbohydrates. Approximately 50 Raman spectra of each substance were acquired per measurement day. A data pipeline was constructed to discover the variability (i.e., instability) of the device for the covered time window. Therein, the stability of the measurement was benchmarked from multiple perspectives, including the intensity variations, the correlation coefficients, the clustering, and the classification. The results suggested the device variability to be more random than systematic. Nonetheless, we demonstrated the possibility of decreasing the variations from the data via computational methods. In particular, we estimated the spectral variations by a network adapted from the variational autoencoder (VAE) and suppressed them from the measured data by the extensive multiplicative scattering correction (EMSC) method. This could improve the prediction of independent measurement days for three representative classification tasks.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"75 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144088111","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-mode colorimetric/photoelectrochemical sensing platform derived from the decomposition of CuHPT for glutathione detection","authors":"Xianwen Kan, Haotian Xue","doi":"10.1039/d5an00410a","DOIUrl":"https://doi.org/10.1039/d5an00410a","url":null,"abstract":"The development of integrated dual signal outputs for reliable and accurate determination of glutathione (GSH) is highly significant for its key role in the physiological processes. Herein, a colorimetric/photoelectrochemical (PEC) dual-mode sensing platform was constructed based on the GSH triggered decomposition of a copper-organic framework (CuHPT). A hollow nanostructured type-II heterojunction of CoS/In-CdS was synthesized using imidazolate framework (ZIF-67) as a template. CuHPT was decomposed in the presence of GSH to form catechol ligands and Cu+, enabling the dual-mode sensing. An ion exchange reaction between the produced Cu+ and Cd2+ of CoS/In-CdS resulted in the formation of Cu2S, causing the decrease of the photocurrent and the sensitive detection of GSH. Cu+ catalyzed H2O2 to produce ·OH via a Fenton-like reaction, achieving the colorimetric sensing. The proposed dual-mode sensor based on the target-triggered decomposition of CuHPT exhibited linear responses for colorimetric and PEC sensing of GSH in ranges of 0.05 - 1.20 mM and 0.5 - 800 μM, with the limit of detections (LODs) of 18 μM and 0.11 μM, respectively. The reliable determination of GSH in human serum provides a new possibility for application of the present dual-mode sensor in clinical assay.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"55 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144066173","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":"Enhancing fouling resistance of graphite sheets for electrochemical sensing of bisphenol-A","authors":"Diele A. G. Araújo, Lauro A. Pradela-Filho, Mariana C. Marra, Thiago C. Oliveira, Allyson L. Rodrigues, Luiz A. J. Silva, Anizio M. Faria, Eduardo M. Richter, Rodrigo A. A. Munoz, Thiago R. L. C. Paixão, Regina M. Takeuchi, André L. Santos","doi":"10.1039/d5an00313j","DOIUrl":"https://doi.org/10.1039/d5an00313j","url":null,"abstract":"Bisphenol A (BPA) is widely used in the production of polycarbonate plastics and epoxy resins, and it is now classified as an emerging pollutant due to its extensive environmental presence. Given the need for effective BPA monitoring, this study presents a cost-effective electrochemical approach for its quantification, using pyrolytic graphite sheets (GSs) as working electrodes integrated into a 3D-printed electrochemical cell. Despite initially exhibiting an intense voltammetric peak for BPA, fouling of the GS surface resulted in a progressive decrease in the BPA signal over successive scans. A pretreatment consisting of applying +1.5 V for 30 s under continuous stirring was adopted before voltammetric measurements. This pretreatment promotes the oxygen evolution reaction, likely cleaning the electrode surface and enhancing its antifouling capability by introducing oxygenated functional groups onto the GS surface. In contrast, this pretreatment was ineffective for a glassy carbon electrode (GCE), likely due to its morphology and reduced reactive surface area, which inhibited the formation of oxygenated functional groups. Under optimized conditions, differential pulse voltammetry with the treated GS electrode yielded a linear range for BPA detection from 0.5 to 1.9 μmol L<small>⁻¹</small>, achieving a detection limit of 0.12 μmol L<small>⁻¹</small>. The proposed electrochemical method was applied to quantify BPA in drinking water and vacuum-pressure mouthguard sheets, providing results statistically equivalent to those obtained using high-performance liquid chromatography. Therefore, this paper presents interesting findings that we believe to be significant for the electroanalysis community, particularly in developing countries where research funding is often limited.","PeriodicalId":63,"journal":{"name":"Analyst","volume":"5 1","pages":""},"PeriodicalIF":4.2,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143980130","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}