Analytica Chimica Acta最新文献

{"title":"Adsorption of fluoroquinolones on hollow Co3S4 polyhedron sulfidated from ZIF-67 and its application of dispersed solid phase extraction prior to HPLC-UV","authors":"Youfang Qi,&nbsp;Xueping Dang,&nbsp;Huaixia Chen","doi":"10.1016/j.aca.2025.344211","DOIUrl":"10.1016/j.aca.2025.344211","url":null,"abstract":"<div><h3>Background</h3><div>Developing pretreatment technique with new adsorbent is essential to improve the detection sensitivity of trace fluoroquinolones (FQs) in complex sample. Zeolite imidazole skeleton-67 (ZIF-67) has adsorbability for FQs, but its structure of rhombohedral dodecahedra may reduce the efficiency of mass transfer, and its application is limited by the instability and poor recyclability.</div></div><div><h3>Results</h3><div>A S-doped hollow Co₃S₄ polyhedron was prepared by sulfidation of ZIF-67 with thioacetamide and applied for disperse solid phase extraction (DSPE) of four FQs. SEM and TEM confirmed its hollow structure, the BET specific surface area was 40.17 m²/g and the adsorption capacity was up to 53.42 mg/g. The adsorption kinetics and isotherm of FQs on the Co₃S₄ polyhedron were investigated. The adsorption process was a chemisorption reaction, which depends on electrostatic interaction, surface complexation, π-π interaction and hydrogen bonding. A DSPE-HPLC-UV method based on the hollow Co₃S₄ polyhedron was developed to determine trace FQs. The method has broad linear range with LODs of 0.10–0.15 μg/kg and LOQs of 0.30–0.50 μg/kg. The intra-batch and inter-batch RSDs were less than 10 %. The recovery rate of FQs in honey samples was satisfactory.</div></div><div><h3>Significance</h3><div>The hollow Co₃S₄ polyhedron has high extraction efficiency for FQs because of the large cavities. Its adsorption capacity was higher than some adsorbents and about 2–3 times than ZIF-67. It has better stability and repeatability. The DSPE-HPLC-UV method based on the hollow Co₃S₄ polyhedron has high sensitivity and is dependable for the determination of trace FQs in complex sample.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344211"},"PeriodicalIF":5.7,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144083350","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Integration of ITO with polyaniline for scalable smart aptasensing interface design: Towards a rainbow assay of Carbamazepine by green Apta-Chip","authors":"Maliheh Arhami ,&nbsp;Alireza Asghari ,&nbsp;Faezeh Shahdost-Fard ,&nbsp;Maryam Rajabi","doi":"10.1016/j.aca.2025.344187","DOIUrl":"10.1016/j.aca.2025.344187","url":null,"abstract":"<div><div>Carbamazepine (CBZ) is an FDA-approved drug for controlling abnormal nerve impulses in the nervous system and brain. Despite the advantages, its overdose causes suicide cases. Close dosage monitoring of CBZ without complex equipment is essential to guarantee its safety and effectiveness from a medicolegal view. This study introduces a novel technology in fabricating the advanced aptasensing interface as the multi-mode Apta-Chip for the electrochemical and visual detection of the CBZ drug in human biofluids based on the green analytical chemistry (GCA) principles. The cornerstone of this study is the integration of the unique electrochromic behavior of polyaniline (PANI) as the sensing platform that undergoes an electric-induced change in coloration and excellent properties of the aptamer (Apt) sequence as the highly selective bioreceptor to CBZ. The molecular dynamic (MD) simulation investigation confirms the conformation changes of the Apt sequence upon incubating CBZ to trap it. The current decrease and resistance increase of the Apta-Chip surface induced by the CBZ/Apt complex forming provides an electrochemical measurement of CBZ by a linear dynamic range (LDR) value from 1 fM to 900 nM and a limit of detection (LOD) value of 333.33 aM. Additionally, different oxidation degrees of PANI in the presence of varying concentrations of CBZ provide a rainbow color switching of the Apta-Chip surface from dark blue to green and yellow colors, corresponding to low, medium and high concentrations, respectively. The utilizing safe and biocompatible chemicals, the unique platform with scalable and miniature size as well as <strong>user-friendliness methodology</strong> in the high selective Apta-Chip fabrication not only guarantee its applicability as the clinical point of care (PoC) device but also offer promising directions that pave the way for progress in other visual home kits for the assay of various analytes.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344187"},"PeriodicalIF":5.7,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144067325","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Precise detection of the low-quality cooking oil by monodisperse droplet generation in a flow-focusing microdroplet generator","authors":"Wen Zeng ,&nbsp;Bohang Wang ,&nbsp;Honglong Chang ,&nbsp;Lomakin Vladimir Olegovich","doi":"10.1016/j.aca.2025.344143","DOIUrl":"10.1016/j.aca.2025.344143","url":null,"abstract":"<div><h3>Background</h3><div>To precisely and efficiently detect the low-quality cooking oil is of great importance to guarantee the food safety in our daily life. Due to the complexity of its origin, the convenient and effective detection methods are still under research.</div></div><div><h3>Results</h3><div>In a flow-focusing microdroplet generator, a new method is provided to detect the low-quality cooking oil based on droplet microfluidics. By controlling the driving pressure of the continuous and the disperse phase, monodisperse water-in-oil droplets can be formed in the flow-focusing microchannel. In particular, as the droplet size is varying with the fluid viscosity and the viscosity of the low-quality cooking oil is different from that of the high-quality cooking oil, therefore, various types of the edible oil samples can be distinguished by measuring the droplet size. Especially by using the method of image processing, the size of the droplets can be measured accurately in the flow-focusing microchannel, which can significantly improve the detection accuracy of the low-quality cooking oil.</div></div><div><h3>Significance</h3><div>In particular, for a specific design of the flow-focusing microdroplet generator, this new method can also provide high reliability for the detection of the deep refined cooking oil based on droplet microfluidics.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1363 ","pages":"Article 344143"},"PeriodicalIF":5.7,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144083355","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Luxuriant Foliage: High-Sensitivity detection of saxitoxin using an enzyme-assisted double-cycling amplification SERS aptamer sensor","authors":"Xiaofan Liu,&nbsp;Xinna Bai,&nbsp;Ziyang Song,&nbsp;Jiekun Zeng,&nbsp;Weicai Wang,&nbsp;Xuemei Li","doi":"10.1016/j.aca.2025.344213","DOIUrl":"10.1016/j.aca.2025.344213","url":null,"abstract":"<div><h3>Background</h3><div>Saxitoxin (STX), one of the most toxic marine toxins known, poses severe risks to marine ecosystems and human health through contaminated seafood. Effective monitoring of STX is critical for early red tide warnings, marine conservation, and food safety. However, existing detection methods often lack sufficient sensitivity or require complex protocols, limiting their practicality for rapid on-site analysis. Therefore, there is a pressing need for a reliable and user-friendly strategy to detect trace levels of STX in the marine environment and to improve the accuracy of these measurements.</div></div><div><h3>Results</h3><div>This study designed an enzyme-assisted double-cycling amplification surface-enhanced Raman scattering (SERS) aptamer sensor for specific and sensitive detection of STX. With the introduction of Nb.BbvCI and Klenow fragment polymerase (KFP), both the target and its aptamer complementary strand achieved double cycling in the system. Meanwhile, the released DNA fragments triggered hybridization chain reaction (HCR), generating a dendritic network for Raman-enhanced detection of STX. All the results showed that the double-cycling amplification SERS aptamer sensor had good recovery rate and high accuracy through enzyme-assisted recycling of the target and its aptamer, and could be used for STX detection in real samples. It is worth noting that the limit of detection (LOD) was calculated to be 1.15 pM according to the 3σ rule, and it has good repeatability when detecting STX.</div></div><div><h3>Significance</h3><div>The enzyme-assisted double-cycling amplification strategy is simple to operate and convenient to separate, improving the sensitivity and selectivity of STX detection, it holds great potential in the field of detecting red tide toxins. Additionally, the strategy's modular design could be adapted to detect other toxins, broadening its impact in environmental and food safety fields.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344213"},"PeriodicalIF":5.7,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144067498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A novel Zn2+ probe for fluorescent monitoring of drug and E6/E7 protein interaction in living cells","authors":"Zhenzhen Xie ,&nbsp;Lan Yu ,&nbsp;Zuoping Li ,&nbsp;Na Zhao ,&nbsp;Shiwan You ,&nbsp;Zhihao Zhao ,&nbsp;Jindi Dou ,&nbsp;Xiling Deng ,&nbsp;Shiguo Sun","doi":"10.1016/j.aca.2025.344202","DOIUrl":"10.1016/j.aca.2025.344202","url":null,"abstract":"<div><h3>Background</h3><div>The zinc-binding sites within the human papillomavirus (HPV) E6/E7 oncoproteins play a critical role in maintaining structural stability and represent promising therapeutic targets due to their cysteine-mediated Zn²⁺ coordination. Zn²⁺ dissociation from these sites serves as a key indicator of direct drug-protein interactions. However, evaluating such interactions is challenging, as E6/E7 proteins localize in the nucleus, necessitating probes capable of traversing both cellular and nuclear membranes while retaining target specificity and real-time monitoring capabilities under physiological conditions.</div></div><div><h3>Results</h3><div>A nuclear membrane-permeable Zn²⁺ fluorescent probe, <strong>NTAD-N2</strong>, was developed for real-time monitoring of Zn²⁺ dynamics in living SiHa cervical cancer cells. This probe-based method was used to evaluate drug efficacy in inducing Zn²⁺ release from HPV16 E6/E7 proteins. Extracellular assays showed disulfiram surpassed ebselen in releasing Zn²⁺ from recombinant proteins. Intracellularly, ebselen induced significant Zn²⁺ release at 5 μM, while disulfiram required 60 μM. This extracellular/intracellular difference in drug efficacy suggests that the bioavailability of disulfiram was influenced by the complex intracellular microenvironment. Specificity was verified through the use of HPV-negative C33A cells as a negative control, where no Zn²⁺ release was detected. Western blot analysis demonstrated that disulfiram-induced Zn²⁺ release at 60 μM resulted from E6/E7 protein degradation, establishing that intracellular Zn²⁺ accumulation originated specifically from E6/E7 protein destabilization.</div></div><div><h3>Significance</h3><div>This study established a novel approach to evaluate zinc-site-targeting drug candidates in live-cell systems, bridging the gap between molecular targeting and cellular efficacy. Furthermore, it underscores the therapeutic potential of disrupting zinc coordination in viral oncoproteins, offering a framework for developing precision interventions against HPV-associated malignancies. This strategy may accelerate the discovery of metalloprotein-targeted therapies for viral infections and related cancers.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1363 ","pages":"Article 344202"},"PeriodicalIF":5.7,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144067510","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A portable instrument-assisted and dual-model sensor array with distinguished color change for the point-of-care identification of tetracycline antibiotics","authors":"Wenhao Li ,&nbsp;Shenghao Meng ,&nbsp;Junxia Wang ,&nbsp;Manman Wang ,&nbsp;Yu He","doi":"10.1016/j.aca.2025.344196","DOIUrl":"10.1016/j.aca.2025.344196","url":null,"abstract":"<div><h3>Background</h3><div>The development of a facile sensor array for the identification of multiple tetracyclines (TCs) is highly promising, considering their similar chemical structures and the associated challenges to public health and food safety. Herein, we explored a dual-model sensor array (ratiometric fluorescence and colorimetric method) for detection and identification of multiple TCs.</div></div><div><h3>Results</h3><div>Three types of ratiometric fluorescent probes based on blue carbon dots (Mg,N-CDs): Mg,N-CDs/MOF-5, Mg,N-CDs/Eu-MOFs, and Mg,N-CDs/Eu-MOFs@Rh-6G, were synthesized as sensing elements. Based on a multi-channel strategy involving the changed signals of the sensing elements, all three probes were able to generate multi-signal fluorescence responses. Under a 365 nm UV lamp, these fluorescence responses were accompanied by obvious color changes (blue to green, blue to red, yellow to red), providing an efficient strategy for on-site quantitative analysis of TCs, including tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC), metacycline (MTC), doxycycline (DOX), and doxycycline hyclate (DTC). A handheld portable 3D-printed platform was also constructed to further enhance the convenience and practicality of detection. This platform utilized the unique ratiometric fluorescence and visual responses of the probes to generate different “fingerprints” for each TC. Effective detection and identification of TCs and their mixtures were achieved by linear discriminant analysis (LDA) and hierarchical cluster analysis (HCA).</div></div><div><h3>Significance</h3><div>The sensitivity of the sensor array based on color change of ratiometric fluorescence was much higher than that of the conventional colorimetric sensor array. Thus, this method not only enriches the techniques for detection of TCs, but also introduces a low-cost, high-performance, dual-model detection tool for on-site analysis.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1363 ","pages":"Article 344196"},"PeriodicalIF":5.7,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143979936","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Interval resonance analysis (InRA): A versatile tool for automated untargeted 1H NMR fingerprinting – A case study in sugar beet field authentication","authors":"Cristian A. Fuentes ,&nbsp;David Montoya ,&nbsp;Mecit Öztop ,&nbsp;Macarena Rojas-Rioseco ,&nbsp;Martin Bravo ,&nbsp;Francisca González ,&nbsp;Rosario del P. Castillo","doi":"10.1016/j.aca.2025.344175","DOIUrl":"10.1016/j.aca.2025.344175","url":null,"abstract":"<div><h3>Background</h3><div>The extraction of relevant information from proton nuclear magnetic resonance (¹H NMR) spectra through preprocessing and multivariate analysis requires integrating multiple software tools and extensive manual intervention, compromising efficiency and reproducibility when the technique is used. Consequently, the development of automated, versatile, and reliable methodologies has become imperative to streamline workflows, improve analytical performance, and broaden the applicability of multivariate methods for the analysis of diverse sample types and experimental conditions.</div></div><div><h3>Results</h3><div>This work presents the development and application of Interval Resonance Analysis (InRA), an alternative software tool focused on ¹H NMR multivariate analysis. InRA includes a novel algorithm for resonance signal detection (intervals), specifically designed to operate with flexibility across diverse ¹H NMR spectra. All intervals are integrated using multivariate curve resolution with alternating least squares (MCR–ALS) and analyzed by exploratory analysis. The performance of InRA was tested by evaluating the ¹H NMR spectra of hydrophilic sugar beet root extracts cultivated in three different fields and their discrimination by partial least squares – discriminant analysis (PLS–DA). The workflow provided by InRA yielded consistent results regarding the distribution of samples according to their field, enabling the identification of subtle sources of variation and achieving classification accuracies ≥ 88.9 %.</div></div><div><h3>Significance</h3><div>The proposed methodology represents an advancement in the multivariate analysis of ¹H NMR spectra for untargeted studies and enhances analytical efficiency by reducing manual intervention and reliance on analyst experience. InRA is versatile and can be applied to various sample types and analytical objectives, as it is not restricted by specific experimental conditions.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1363 ","pages":"Article 344175"},"PeriodicalIF":5.7,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143979937","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Unsupervised classification of iron ores based on elemental and isotopic signatures from atomic and molecular emissions of laser-induced plasma","authors":"Sung-Uk Choi ,&nbsp;Sol-Chan Han ,&nbsp;Jong-Il Yun","doi":"10.1016/j.aca.2025.344191","DOIUrl":"10.1016/j.aca.2025.344191","url":null,"abstract":"<div><h3>Background</h3><div>Iron ore classification by grade and origin is critical for quality assurance in steel manufacturing. However, traditional analytical methods can be time-consuming and may not provide comprehensive information for accurate classification.</div></div><div><h3>Results</h3><div>The present study introduces a novel classification approach utilizing laser-induced breakdown spectroscopy (LIBS) to simultaneously discriminate iron ore grades (fine, lump, and concentrate) and origins (Australia, Brazil, and South Africa), without necessitating prior knowledge of the samples. A key aspect of this approach is to leverage multiple spectral features from laser-induced plasma: (i) atomic lines representing elemental composition, and (ii) molecular bands reflecting isotopic signatures. Based on this comprehensive spectral data, principal component analysis (PCA) was employed to visualize the correlations among the datasets, thereby illustrating how elemental composition and isotopic abundance correlate with grades and origins. Subsequently, the <em>k</em>-means clustering algorithm was utilized as an unsupervised classifier, eliminating the need for previously labeled training data. Consequently, the present approach could achieve an accuracy exceeding 94 % in determining the grade and origin of ores.</div></div><div><h3>Significance</h3><div>This study successfully established the rapid and versatile classification method for unknown iron ores, offering significant benefits for various industrial applications.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344191"},"PeriodicalIF":5.7,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144066494","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Biological sample desalting and buffer replacement based on electromigration in a discontinuous electrolyte system using a 3D printed device","authors":"Vanda Kocianová ,&nbsp;Ivona Voráčová ,&nbsp;Yann Astier ,&nbsp;Doo Soo Chung ,&nbsp;František Foret","doi":"10.1016/j.aca.2025.344198","DOIUrl":"10.1016/j.aca.2025.344198","url":null,"abstract":"<div><h3>Background</h3><div>The quality and yield of DNA specimens are essential for downstream analyses. Complex biological or environmental samples contain interfering compounds requiring advanced protocols for removing salts, small organic molecules, and/or proteins without compromising the DNA fragments distribution in the original sample. High-molecular-weight DNA fragments are often discriminated by standard extraction methods in attempts to remove the highly concentrated inorganic sample components.</div></div><div><h3>Results</h3><div>Here, we introduce a simple device for the simplification, purification, desalting, and buffer exchange of complex biological samples based on electrodialysis in discontinuous electrolyte systems. The device combines a 3D-printed body with two electrolyte reservoirs and commercially available cassettes with dialysis membranes as inserts. Upon applying an electric current via electrodes inside the electrolyte reservoirs, the sample ions, injected into the cassette or one of the electrolyte reservoirs, electromigrate across the dialysis membranes. During this process, small sample ions pass through the membrane and are substituted by the ions of the selected buffers loaded into the electrolyte reservoirs. The larger ions, such as DNA fragments or proteins, stay in the sample reservoir. The performance of the device was evaluated using DNA samples in blood plasma. Several milliliters of a plasma sample were purified in 30 min with 90 % DNA recovery.</div></div><div><h3>Significance</h3><div>The device enables fast and effective purification of highly complicated samples. It can be easily scaled for the available sample amount (ranging from microliters to milliliters) and the analyte size of interest by selecting appropriate membrane pore sizes. The device's applicability was optimized on DNA samples with high salt content and tested on plasma samples. But it also has the potential for purification/desalting of a wide range of biological compounds, including proteins, peptides, or charged oligosaccharides, as well as organelles, cells, viruses, or bacteria.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1364 ","pages":"Article 344198"},"PeriodicalIF":5.7,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144066490","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Advancing NMR-based quantification in complex mixtures using fourier transform and complete reduction to amplitude frequency table - The case of sugars","authors":"Jennifer Janovick ,&nbsp;Krish Krishnamurthy ,&nbsp;Peter Howard ,&nbsp;Emmanuel Hatzakis","doi":"10.1016/j.aca.2025.344173","DOIUrl":"10.1016/j.aca.2025.344173","url":null,"abstract":"<div><h3>Background</h3><div>Sugars are building blocks of polysaccharides, and they are involved in many food and biotechnological applications. However, current methods of analysis have several limitations, preventing our understanding about their functions and roles in different systems, such as biological mixtures. Thus, there is a constant need for analytical methods that allow their rigorous and convenient quantification. NMR-based methodologies have a great potential in sugar analysis, however the traditional Fourier transform approach is associated with significant challenges related to sensitivity, resolution and error prone processing steps.</div></div><div><h3>Results</h3><div>A “clean” and straightforward ¹³C-detected NMR method for sugar analysis was developed. Nine sugars commonly found as building blocks of polysaccharides were analyzed with ¹H and ¹³C NMR with the later found to be more effective due to the complexity of the mixtures. Minor tautomers were also identified and found to appear in relatively significant amounts in some cases. In addition to the traditional Fourier transform, integration-based approaches, CRAFT-based analysis was assessed for the quantification of sugars in a complex mixture. CRAFT utilizing Bayesian analysis was found to generate high quality and repeatable results in an automated and less error-prone manner. Finally, CRAFT allows for significant improvement in spectral resolution of the 2D HSQC, thus rendering the NMR assignment much more convenient, even for less experience users.</div></div><div><h3>Significance</h3><div>This novel and systematic study for the quantification of sugars in complex mixtures with Fourier transform and CRAFT, will advance our capabilities for sugar quantification. It is also expected to lay the groundwork for the application of time-domain NMR data for targeted analysis and can be extended to other matrices.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1363 ","pages":"Article 344173"},"PeriodicalIF":5.7,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143979966","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}