Analytica Chimica Acta最新文献

{"title":"Expanding time-resolved ICP-MS capabilities for characterizing cells and biogenic nanoparticles in hypersaline media","authors":"Nuria Guijarro-Ramírez ,&nbsp;Raquel González-de Vega ,&nbsp;Iraide Sáez-Zamacona ,&nbsp;Luis Gras ,&nbsp;Rosa María Martínez-Espinosa ,&nbsp;David Clases ,&nbsp;Guillermo Grindlay","doi":"10.1016/j.aca.2025.344731","DOIUrl":"10.1016/j.aca.2025.344731","url":null,"abstract":"<div><h3>Background</h3><div>The analysis of halophilic organisms using time-resolved inductively coupled plasma mass spectrometry (TRA ICP-MS) is challenging due to severe matrix effects caused by the high total dissolved solid concentration (200 g L⁻¹) in their culture media. This work introduces a methodology that overcomes these issues by using <em>Haloferax mediterranei</em> as a model organism. The developed method preserves cell integrity and minimizes matrix effects, which enabled us to investigate Pb bioaccumulation and selenium nanoparticle (SeNP) formation in this archaeon by means of time-resolved inductively coupled plasma time-of-flight mass spectrometry (TRA ICP-TOFMS).</div></div><div><h3>Results</h3><div>To preserve <em>H. mediterranei</em> cells and mitigate matrix effects from high total dissolved solids, TRA ICP-MS working conditions were carefully optimized. A High-efficiency nebulizer and double-pass spray chamber were selected for sample introduction, as this configuration ensured high sensitivity and reduced matrix load into the plasma. Additionally, on-line sample dilution using a T-connector to achieve a 1:10³ ratio and aerosol dilution were implemented to further reduce matrix load and mitigate cell osmotic stress. The method was used to monitor Pb bioaccumulation and detect biogenic SeNPs within individual cells using ICP-TOFMS. Lead and SeNPs detection limits were, respectively, 15 ag cell⁻¹ and 42 nm. Single cell Pb uptake was highly heterogeneous, ranging from 20 to 300 ag cell⁻¹ while SeNP sizes were between 47 and 73 nm. Co-detected events of Pb and Se suggests that SeNPs are located intracellularly rather than being expelled and freely suspended in the medium.</div></div><div><h3>Significance</h3><div>This methodology represents a significant advancement, as it is the first TRA ICP-MS approach to accurately analyze single halophilic cell in hypersaline media without the need for extensive sample preparation. This development allows for the quantitative assessment of heavy metal bioaccumulation and NP formation in extremophiles, thereby extending TRA ICP-MS applicability.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1379 ","pages":"Article 344731"},"PeriodicalIF":6.0,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145195165","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":"Accessing the proteome of extracellular vesicles via rapid acoustic isolation of a minute human blood plasma sample","authors":"Megan Havers ,&nbsp;Aaron M. Scott ,&nbsp;Niklas Ortenlöf ,&nbsp;Charlotte Welinder ,&nbsp;Simon Ekström ,&nbsp;Thierry Baasch ,&nbsp;Mikael Evander ,&nbsp;Andreas Lenshof ,&nbsp;Magnus Gram ,&nbsp;Thomas Laurell","doi":"10.1016/j.aca.2025.344661","DOIUrl":"10.1016/j.aca.2025.344661","url":null,"abstract":"<div><h3>Background</h3><div>Despite substantial progress in the field of mass spectrometry, there remain barriers to measuring the extracellular vesicles (EVs) proteome in blood plasma. Recent work has shown that isolating EVs can make it possible to detect proteins that have low abundance in plasma. Commonly used EV isolation methods either require large sample volumes and long ultracentrifugation times, or else result in population bias via targeted isolation. There is a great need for fast and easy methods to isolate EVs from small volumes of plasma, &lt;10 μL, enabling biomarker discovery, e.g. in biobanked samples, where mass spectrometry can play an important role.</div></div><div><h3>Results</h3><div>We unveil the extracellular vesicle proteome by using seed particle enhanced acoustic trapping to purify EVs from minute blood plasma samples (8 μL) in 6 min per sample. The differential mass spectrometry results find proteins which are significantly enriched (FDR-adjusted p-values&lt;0.05) in acoustically trapped samples compared to raw (unprocessed) plasma, more than two thirds of those proteins have been associated with EVs previously. Additionally, we are able to increase the depth of analysis by detecting 51 low abundance proteins not detected in raw plasma, half of which are tagged with the gene ontology (GO) tag “extracellular exosome” (GO:0070062). Finally, we validate the novel use of neutrally charged silica seed particles paired with a washing flowrate of 200 μL/min, enabling the processing time to be halved and finding the same proteome as for tried-and-tested polystyrene seed particles with washing at 30 μL/min.</div></div><div><h3>Significance</h3><div>Our microfluidics-based approach to EV isolation enables rapid processing of an individual minute blood plasma sample, demonstrating that personal proteomic information associated with EVs can be detected when acoustic trapping is used as a pre-processing step. By applying this technique to plasma from patient cohorts or mouse models, future studies may offer new insights into the role of EVs in the progression of diseases and reveal new diagnostic targets in the proteomic cargo of EVs.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1379 ","pages":"Article 344661"},"PeriodicalIF":6.0,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145203416","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 geochemical analysis and K-means clustering for sustainable management of various dam sediments","authors":"İbrahim Mizan Kahyaoğlu ,&nbsp;Ahmet Uyanık ,&nbsp;Canan Hazal Akarsu ,&nbsp;Tarık Küçükdeniz ,&nbsp;Selcan Karakuş ,&nbsp;Murat Güney","doi":"10.1016/j.aca.2025.344730","DOIUrl":"10.1016/j.aca.2025.344730","url":null,"abstract":"<div><div>Optimizing the use of existing dams can reduce the need for new construction and support sustainable dam management. In this study, key sediment parameters including humic acid (HA), fulvic acid (FA), %C, %H, %N, total organic matter (TOM), pH, conductivity, and shrink/swell capacity were analyzed. Heavy metal concentrations ranged from 1.62 to 7.74 mg/kg (As), 1.40–2.91 mg/kg (Cd), 6.79–18.44 mg/kg (Co), 19.46–85.61 mg/kg (Cr), 21.12–63.60 mg/kg (Cu), 8000–46,500 mg/kg (Fe), 260–1120 mg/kg (Mn), 27.12–180 mg/kg (Ni), 2.52–10.22 mg/kg (Pb), and 30.50–88.10 mg/kg (Zn). Organic material contents were 0.050–0.88 % for HA and 0.01–1.21 % for FA. Measured pH values ranged from 6.99 to 7.92, conductivity from 0.26 to 4.49 mS/cm, and shrink/swell capacity from 34.37 to 54.11 %. The dataset was normalized using Min-Max scaling to ensure consistency and reduce bias. K-means clustering was applied to identify sediment profiles, yielding insights into pollution levels, soil fertility, and retention capacity. The integration of geochemical analysis with artificial intelligence (AI)-based clustering demonstrated the effectiveness of machine learning (ML) methods in classifying sediments based on heavy metal concentrations. Additionally, SEM analysis revealed distinct layered surface properties with nanoglobular structures ranging from 100 nm to less than 10 nm, offering further insights into the sediment characteristics and potential agricultural applications. This study underscores the importance of integrating AI techniques with traditional analyses to enhance sediment characterization and promote sustainable environmental management.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1379 ","pages":"Article 344730"},"PeriodicalIF":6.0,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145195496","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":"Isothermal nucleic acid amplification-based magnetic aptasensor for sensitive detection and in situ imaging of Trop-2 in triple-negative breast cancer","authors":"Wenqing Shao,&nbsp;Xiaoting Liu,&nbsp;Yi Zhou","doi":"10.1016/j.aca.2025.344734","DOIUrl":"10.1016/j.aca.2025.344734","url":null,"abstract":"<div><h3>Background</h3><div>Triple-negative breast cancer (TNBC) is strongly linked to overexpression of Trop-2, a transmembrane glycoprotein biomarker implicated in its aggressive behavior. For in situ imaging and quantification of this membrane protein, we developed a highly sensitive fluorescence aptasensor.</div></div><div><h3>Results</h3><div>Upon recognition of Trop-2 by its specific aptamer, hybridization chain reaction (HCR) was triggered for in situ imaging of cell-surface Trop-2. Concurrently, catalytic hairpin assembly (CHA) amplified fluorescence signals for quantitative Trop-2 detection. Successful cellular imaging and quantitative Trop-2 detection were achieved a linear response was observed from 0.001 μM to 0.1 μM, the limit of detection (LOD) was determined to be 0.0009 μM. Trop-2 surface density measurements revealed average amount per cell of: 6.0 × 10⁶ molecules per cell (MDA-MB-468), 2.0 × 10⁶ molecules per cell (MCF-7), 6.6 × 10⁵ molecules per cell (MDA-MB-231), and 4.1 × 10⁵ molecules per cell (HL-7702).</div></div><div><h3>Significance</h3><div>To our current knowledge, the work represents the first aptasensor enabling both in situ Trop-2 protein imaging and quantitative comparison across diverse cell types. The proposed method shows promise for tumor diagnosis and therapeutic evaluation.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1380 ","pages":"Article 344734"},"PeriodicalIF":6.0,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145203422","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":"Raman and NIR spectroscopy: A discussion of calibration robustness for food quality measurements through two case studies","authors":"Tiril Aurora Lintvedt,&nbsp;Petter Vejle Andersen,&nbsp;Nils Kristian Afseth,&nbsp;Jens Petter Wold","doi":"10.1016/j.aca.2025.344658","DOIUrl":"10.1016/j.aca.2025.344658","url":null,"abstract":"<div><h3>Background:</h3><div>Fast and nondestructive spectroscopic measurements of food quality are of great interest to the food industry due to their huge potential in decision support and optimization of processes and food value chains. Choosing the type of spectroscopic technique to invest in is not always straight-forward. In this work, we discuss the robustness aspect of Raman and NIR spectroscopy as a relevant factor to consider. We hypothesize that Raman spectroscopy has an advantage in calibration development and maintenance due to the higher degree of chemical details in the spectra, lower degree of band overlap and lower sensitivity to water.</div></div><div><h3>Results:</h3><div>Robustness was discussed through two case studies, assessing (1) the transferability of intact strawberry sugar calibrations between seasons and (2) the transferability of fat models between different meat grinding degrees. The work indicates that Raman spectroscopy has an inherent chemometric advantage for robustness. This was particularly pronounced in the strawberry case, where Raman models of around half the complexity (number of PLSR components) of NIR-based models reached similar performances and provided more interpretable regression vectors. The meat case demonstrated that the robustness of the techniques may depend on the sensitivity to different sample textures and heterogeneity. A Raman probe with a spot size of 3 mm diameter suffered from higher prediction errors than a probe with 6 mm diameter spot size. We also demonstrated an additional challenge of increasing fluorescence with longer meat storage time for Raman spectroscopy. Still, a Raman system with 6 mm spot size outperformed a reflection geometry NIR system with approximate illumination spot of 1 cm.</div></div><div><h3>Significance:</h3><div>Few studies that compare Raman and NIR spectroscopy within food applications, focus on the differences regarding robustness. This work shows that the cost of developing and maintaining a calibration industrially should be considered to a higher extent and be part of the evaluation on final cost and implementation ease, when deciding between Raman and NIR spectroscopy or what type of sampling optic to invest in. The findings should motivate critical comparisons of the two techniques prior to long-term sensing implementation.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1379 ","pages":"Article 344658"},"PeriodicalIF":6.0,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145195497","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":"Machine learning-assisted retention time predictions on a cellulose Tris(3,5)-dimethylphenylcarbamate column in polar organic mode","authors":"Attila Imre ,&nbsp;Gergely Dombi ,&nbsp;Máté Dobó ,&nbsp;Ali Mhammad ,&nbsp;Elek Ferencz ,&nbsp;Balázs Balogh ,&nbsp;Anna Vincze ,&nbsp;Zoltán-István Szabó ,&nbsp;György Tibor Balogh ,&nbsp;Anita Rácz ,&nbsp;Gergő Tóth","doi":"10.1016/j.aca.2025.344733","DOIUrl":"10.1016/j.aca.2025.344733","url":null,"abstract":"<div><h3>Background</h3><div>Enantioseparation in HPLC is a considerable challenge in analytical chemistry, frequently requiring numerous trials with varying experimental conditions to achieve baseline separations. To address this issue, we propose a solution that utilizes consensus modelling based on partial least squares (PLS) regression method together with neural network (NN) algorithms and a graph neural network (GNN) method to predict the retention times of compounds on Lux Cellulose-1 chiral stationary phase under various polar organic mode mobile phases.</div></div><div><h3>Results</h3><div>A homogeneous dataset was collected for the developed machine learning methods, consisting of 535 unique molecules and 1,414 retention time measurements under four polar organic mode conditions (acidic and basic methanol, acidic and basic acetonitrile). The PLS + NN consensus model showed outstanding results in condition-specific predictions, achieving R² values over 0.70 and RMSE values below 0.40 in most cases. Conversely, the GNN model excelled in combined predictions under all conditions, achieving a R² of 0.58 and RMSE_CV of 0.49 during cross-validation, as well as a R² of 0.85 and RMSE_Test of 0.25 on the test set.</div></div><div><h3>Significance</h3><div>Our research presents a novel approach for predicting chiral separations, offering an easy-to-use, open-access web tool to the scientific community. The robust GNN model was used to create a web server (<span><span>https://chiralscreen.com</span><svg><path></path></svg></span>) that enables the prediction of retention times, separation capabilities, and elution orders for various compounds. Furthermore, the software helps determine optimal initial chromatographic conditions for separations.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1379 ","pages":"Article 344733"},"PeriodicalIF":6.0,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145195208","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":"Intelligent multi-index urine detection using colorimetric hydrogel for integrated urinary tract infections diagnosis","authors":"Ying Gao ,&nbsp;Haiqin Li ,&nbsp;Xiaochun Li","doi":"10.1016/j.aca.2025.344729","DOIUrl":"10.1016/j.aca.2025.344729","url":null,"abstract":"<div><h3>Background</h3><div>Urinary tract infection (UTI) is a significant global health issue. Urine bacterial culture is time-consuming, prone to misdiagnosis, and the existing sample pretreatment methods are cumbersome, relying on centralized laboratories and specialized equipment. Colorimetric sensing provides a faster alternative. However, its accuracy is often compromised by the variable color of the patient's urine samples. Therefore, it is clear that a rapid, simple, gentle, and environmentally friendly pretreatment method is needed that effectively eliminates color interference in colorimetric detection and is compatible with smartphones, enabling real-time, quantitative on-site monitoring of UTI. (90)</div></div><div><h3>Results</h3><div>In this study, we describe a unique smartphone-assisted diagnostic method for quantifying nitrite, leukocyte esterase (LE), and bacteria in urine samples. The method employs activated carbon composite hydrogel spheres for urine pretreatment, which effectively removes background color interference and improves sensor performance, and combined with a smartphone-based microplate analyzer independently developed by our group previously, allows for precise colorimetric examination. This will aid in the prompt detection and dynamic monitoring of urinary tract infections in clinical settings. Furthermore, the bacterial detection time was shortened to 2 h, enhancing the accuracy and timeliness of the diagnostic process. The detection limits of nitrite, LE, and <em>E. coli</em> were 0.0584 mg L⁻¹, 0.0775 Leu μL⁻¹, and 2.94 CFU mL⁻¹, respectively, meeting clinical requirements. Validation of 147 clinical samples indicated high consistency with the Sysmex UC-3500 Automatic Urine Analyzer, demonstrating the sensor's durability and accuracy. (141)</div></div><div><h3>Significance</h3><div>Activated carbon hydrogel beads with high adsorption properties were used for the pretreatment of urine samples for the first time, effectively removing background color interference in colorimetric detection. Integration of a smartphone-based microplate analyzer with a hydrogel slow-release system enables quantitative detection of nitrite, LE, and bacteria. This strategy offers a portable, low-cost solution for home-based UTI monitoring, enabling more timely management and appropriate administration of therapy to improve patient outcomes. (71)</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1379 ","pages":"Article 344729"},"PeriodicalIF":6.0,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145195157","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":"Hydrophobic magnetic deep eutectic solvents: An all-in-one platform for fast visualization, removal, recycle and degradation of anionic dyes","authors":"Yanshang Kang ,&nbsp;Yangrui Si ,&nbsp;Qiwen Jin ,&nbsp;Ruohan Xu ,&nbsp;Yujun Zhong ,&nbsp;Yaorui Wang ,&nbsp;Yuxiang Fu ,&nbsp;Jing Gu ,&nbsp;Mingfu Ye ,&nbsp;Shuangshou Wang","doi":"10.1016/j.aca.2025.344725","DOIUrl":"10.1016/j.aca.2025.344725","url":null,"abstract":"<div><h3>Background</h3><div>With the wide use of dyes, the issues they caused in food safety and environmental pollution have become increasingly serious. Endeavors for dyes detection, removal, recycling and degradation are of great significances. However, existing methods for dyes detection are highly relied on instrumental tools. High instrumentation cost and poor portability prevent them being used for on-site rapid detection. For separation, recycling and degradation of dyes, well-designed materials featured with fine-tunable pore size, good permeability and large specific surface area are often indispensable. Robust and user-friendly multi-function platforms are highly practical but still rather limited.</div></div><div><h3>Results</h3><div>An all-in-one platform for fast visualization, removal, recycle and degradation of anionic dyes was developed using hydrophobic magnetic deep eutectic solvents (HMDESs) as an all-rounder. Anionic dyes could be efficiently extracted by HMDESs through electrostatic interaction and hydrophobic effect, giving extraction rates over 99.0 % within 3 min. Colorimetric assays were adopted for fast visualization of dyes, of which the colorimetric LODs reached 10⁻⁷ g/mL level. The extracted dyes could be facilely desorbed and recycled via adjusting system pH, showing recycling rates surpassed 99.5 %. By combining with H₂O₂, Fenton reactions constructed by Fe³⁺-doped HMDES achieved nearly complete degradation of the extracted dyes. As proof-of-concept assays, the multi functions of HMDESs were experimentally proved using commercial drinks and simulated dye effluents (viz., dyes-spiked purified water, tap water, river water, aquaculture pond water and industrial sewage) as real samples, and the results were double-verified with instrumental tools and smartphone-derived digital image analysis.</div></div><div><h3>Significance</h3><div>A HMDESs-based multi-purpose platform has been constructed herein, and its applications for fast visualization, removal, recycle and degradation of anionic dyes in both food and environmental samples have also been demonstrated. As far as we know, this is the first case to report such an all-in-one platform constructed by HMDESs for multi-dimension analysis of dyes. Since HMDESs are of many merits such as fine transplantability, easy-to-prepare, low cost, handy magnetic separation, etc., this work will find its more potentials in other areas like environmental analysis and biochemical separation and offer a reference for design other platforms for multi-use applications.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1379 ","pages":"Article 344725"},"PeriodicalIF":6.0,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145195498","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":"Development of a robust sulfo-phospho-vanillin assay for sample normalization in LC-MS-based lipidomics","authors":"Fernanda Sousa Monteiro ,&nbsp;Adriana Zardini Buzatto ,&nbsp;Liang Li","doi":"10.1016/j.aca.2025.344652","DOIUrl":"10.1016/j.aca.2025.344652","url":null,"abstract":"<div><h3>Background</h3><div>Lipidomics, the comprehensive analysis of lipid profiles in biological samples, is crucial for understanding cellular processes and disease mechanisms. However, variations in the amounts or concentrations of samples can significantly impact the accuracy of lipid quantification in comparative studies. To address this challenge, the normalization of samples before processing and analysis is essential. This study introduces a robust normalization method for lipidome analysis, leveraging an improved sulfo-phospho-vanillin (SPV) analysis technique.</div></div><div><h3>Results</h3><div>The enhanced SPV method provides a reliable colorimetric assay for determining total lipid content across diverse sample types. By optimizing the detection limits and reducing the required sample amount for the assay, we successfully applied this method to saliva and cellular samples where the concentrations of the starting materials can have large variations. Our findings demonstrate that SPV normalization significantly improves lipid feature detection and intensity consistency across samples without introducing analytical bias. This normalization process facilitates more accurate comparisons of lipid profiles.</div></div><div><h3>Significance</h3><div>Implementing SPV-based normalization presents a practical solution for enhancing the accuracy of lipidome analyses in comparative studies. This approach is not only effective but also accessible for research laboratories, requiring a relatively simple workflow and standard UV–visible spectroscopy equipment.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1378 ","pages":"Article 344652"},"PeriodicalIF":6.0,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145218859","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":"At-line determination of the enantiomeric excess in multi-component chiral samples using Raman optical activity (ROA)","authors":"Karolina Kwiecień ,&nbsp;Piotr Putyra ,&nbsp;Agnieszka Kaczor","doi":"10.1016/j.aca.2025.344727","DOIUrl":"10.1016/j.aca.2025.344727","url":null,"abstract":"<div><h3>Background</h3><div>Enantiomerically pure drugs offer better specificity, higher therapeutic index, and optimized pharmacokinetics compared to racemic drugs. However, pharmaceutical companies continue manufacturing racemic medicines, among others, due to the lack of tools for <em>in situ</em> determination of the optical purity and the absolute configuration, which is necessary for approval of drug substance by the European Medicines Agency (EMA) or the US Food and Drug Administration (FDA). Currently used methods for the absolute configuration and the enantiomeric excess determination have significant limitations (require single crystal, UV-active chromophores, chiral reagents, etc).</div></div><div><h3>Results</h3><div>Addressing this need of pharmacological industry for the effective analysis of chiral drugs <em>in situ</em> in solution, we have designed and constructed the at-line setup based on Raman optical activity (ROA) and equipped with the 3D-printed flow reactor dedicated for fast <em>in situ</em> and in-flow analysis of chiral compounds. We have validated our approach by the determination of the enantiomeric excess (EE) of pure and multi-component chiral samples showing that the developed solution combines the excellent stereosensitivity, possibility to measure chiral samples in-flow, and a rather unique capability of direct discrimination of components of chiral mixtures. The quantitative analysis based on Partial Least Squares (PLS) regression has demonstrated that the accuracy and precision of the method is very high with the average prediction error from cross-validation (RMSECV) not exceeding 1.35 % (for R² at least 99.95) for ROA spectra recorded in 20 min.</div></div><div><h3>Significance</h3><div>According to our best knowledge, our work is a first example of successful in-flow and <em>in situ</em> ROA evaluation of chiral purity in chiral mixtures. Our direct approach does not require extensive sample preparation, preliminary separation of enantiomers or derivatization. In the long-term, our solution paves the way toward operando (in-line) ROA, enabling real-time monitoring of chirality in reaction mixtures.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1379 ","pages":"Article 344727"},"PeriodicalIF":6.0,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145188822","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}