Zehra Tuğçe Kurt, Handan Yavuz Alagöz, Nilay Bereli
{"title":"The role of electrochemical and optical biosensors in the detection of chemical and biological agents: a critical review.","authors":"Zehra Tuğçe Kurt, Handan Yavuz Alagöz, Nilay Bereli","doi":"10.1007/s00216-025-06162-x","DOIUrl":"https://doi.org/10.1007/s00216-025-06162-x","url":null,"abstract":"<p><p>The increasing risk associated with chemical and biological warfare agents has amplified the need for rapid, sensitive, and portable detection technologies, particularly in the context of CBRN (chemical, biological, radiological, and nuclear) threats. While conventional analytical techniques such as high-performance liquid chromatography, gas chromatography/mass spectrometry, and the polymerase chain reaction remain the gold standard for analytical accuracy, they are often hindered by high operational costs, complex instrumentation, and limited field applicability. In response, biosensor technologies have emerged as promising alternatives, offering advantages such as real-time analysis, portability, and cost-effectiveness. This critical review provides a comparative evaluation of recent advances in electrochemical and optical biosensor platforms for detecting CBRN-relevant chemical and biological agents. The performance of each platform is analyzed in terms of sensitivity, specificity, operational stability, and environmental robustness. Electrochemical biosensors demonstrate strong potential for on-site applications due to their low cost and adaptability, whereas optical biosensors exhibit exceptional sensitivity and multiplexing capabilities, though with certain limitations in terms of portability and environmental resilience. Selected case studies are discussed to highlight prevailing design strategies, material innovations, and detection principles. Moreover, current challenges are identified, including the lack of standardized validation protocols, limited multi-analyte detection capabilities, and insufficient field testing. The review concludes by outlining future perspectives, emphasizing the importance of integrating artificial intelligence, sustainable materials, and modular sensor designs to enhance real-world applicability in diverse and unpredictable CBRN scenarios.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145342527","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}
Toni Köppe, Nina Hermes, Kevin S Jewell, Arne Wick, Sylvia Rohde, Thomas A Ternes
{"title":"A category approach to characterize river sites based on non-target screening and target analysis.","authors":"Toni Köppe, Nina Hermes, Kevin S Jewell, Arne Wick, Sylvia Rohde, Thomas A Ternes","doi":"10.1007/s00216-025-06124-3","DOIUrl":"https://doi.org/10.1007/s00216-025-06124-3","url":null,"abstract":"<p><p>The objective of this study was to characterize monitoring sites with regard to their contaminating sources and to identify potential pollution hotspots as well as previously unknown compounds. Several evaluation methodologies were combined via a category approach consisting of site-specific detections using a combination of an extended target analysis via GC/MS and LC/MS/MS, NTS using LC-reversed phase high resolution MS, and suspect screening via spectral libraries. Furthermore, we considered the fraction of treated wastewater, the agricultural land use, and industry located in the vicinity. In order to evaluate our concept, more than 520 water samples of rivers from 79 locations throughout Saxony were analyzed by target analysis and NTS. Overall, a very good comparability between the results of target analysis and NTS was observed for pharmaceuticals and pesticides. In a first step, NTS data were used to identify hotspots of pollution with organic micropollutants. By this approach, 13 of 79 sites were characterized as \"anomalous\" as defined by empirical thresholds. More than 350 compounds could be identified using our spectral data library. In a second step, features of two sampling sites, which were likely contaminated by treated industrial wastewater, were investigated in detail, leading to the identification of four currently unknown compounds. These were cyclohexyldiethanolamine (CDA), 2,4,6-tri-(6-amino-hexanoic acid)-1,3,5-triazine (THAT), 2-(dibutylamino)ethanol, and 3,6,9-trioxaundecanedioic with estimated concentrations of up to 100 µg/L in rivers and streams using a semi-quantitative approach. However, based on the NTS database obtained, the identification of further currently unknown compounds can be easily done. The suggested category approach was also suitable to identify pollution hotspots of organic chemicals.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145342542","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}
Nho-Eul Song, Jeonghyun Yun, Sunhee Kang, Jang-Eun Lee
{"title":"Optimized method for analyzing volatile compounds in edible yeast using headspace SPME-GC-MS.","authors":"Nho-Eul Song, Jeonghyun Yun, Sunhee Kang, Jang-Eun Lee","doi":"10.1007/s00216-025-06153-y","DOIUrl":"https://doi.org/10.1007/s00216-025-06153-y","url":null,"abstract":"<p><p>Volatile compounds produced by edible yeasts play a critical role in food flavor and consumer perception. This study aimed to evaluate how different yeast preparation methods influence the detection of volatile compounds using gas chromatography-mass spectrometry (GC-MS) coupled with headspace solid-phase microextraction (HS-SPME). Saccharomyces cerevisiae was prepared using four methods-broth culture, agar culture, supernatant, and yeast cell pellet-and volatile profiles were compared with non-polar (DB-5), mid-polar (DB-17), and polar (VF-WAX) GC columns. The supernatant consistently exhibited the greatest diversity and abundant volatile compounds, whereas agar cultures and cell pellets led to fewer volatiles. Principal component analysis (PCA) demonstrated distinct clustering of volatile profiles according to the preparation method, with major compounds such as hexanoic acid ethyl ester and phenylethyl alcohol contributing to group separation. Additionally, the effect of salting-out agents (NaCl and H<sub>2</sub>NaPO<sub>4</sub>) on volatiles extraction efficiency was examined, showing that NaCl led to increased levels of alcohols, while H<sub>2</sub>NaPO<sub>4</sub> enhanced acid extraction. These findings underscore the importance of optimizing sample preparation conditions, column polarity, and extraction parameters for accurate and reproducible analysis of yeast-derived volatiles. The results provide practical insights into targeted flavor profiling and the development of yeast-derived flavor applications in the food and fermentation processes.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145342492","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":"Automated vortex-assisted-liquid-liquid microextraction with injector-based derivatization for GC-MS/MS analysis of 1,3-dichloropropan-2-ol and 3-chloropropane-1,2-diol in food contact paper products.","authors":"Malte Hübschen, Fabrian Brenz, Torsten C Schmidt","doi":"10.1007/s00216-025-06133-2","DOIUrl":"https://doi.org/10.1007/s00216-025-06133-2","url":null,"abstract":"<p><p>The analysis of 1,3-dichloropropan-2-ol (1,3-DCP) and 3-chloropropane-1,2-diol (3-MCPD) in paper products and cardboard boxes used as food contact materials is of great importance due to the potential health risks associated with the intake of these contaminants. Both compounds, which originate from wet strength agents used in paper production, pose significant health concerns: 1,3-DCP and 3-MCPD are classified as possibly carcinogenic to humans and suspected to be carcinogenic in humans, respectively. This study presents a novel, automated analytical method for the analysis of a cold water extract-a widely used procedure for isolating these analytes from paper products and cardboard boxes. Method development included the implementation of vortex-assisted liquid-liquid microextraction (VALLME) with a focus on reducing solvent consumption and improving environmental sustainability and the systematic investigation of derivatization techniques. Optimization of the extraction solvent, extraction time, and derivatization parameters using vial-based and injector-based approaches resulted in a lean and rapid method with low limits of detection (0.01 µg/L for 1,3-DCP and 0.16 µg/L for 3-MCPD). The method showed good precision with intra-day repeatabilities of 3.6-3.7% for 1,3-DCP and 3.6-5.9% for 3-MCPD and inter-day repeatabilities of 2.6-3.6% and 4.0-7.6%, respectively. Recoveries ranged from 100 to 102% for 1,3-DCP and from 90 to 99% for 3-MCPD. Comparative assessment with a reference method confirmed good precision and comparability of the method. Improved environmental performance was quantified by the analytical greenness metric for sample preparation.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145336131","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":"Core-shell Au@4-MBA@Ag enhanced SERS immunochromatography for rapid and on-site detection of deoxynivalenol in animal feeds.","authors":"Xinyi Song, Zhaoyuan He, Siyuan Tan, Siyu Cong, Wuli Lu, Zedeng Mai, Mingsheng Jiang, Yu Wen, Cheng Liu, Hailan Chen","doi":"10.1007/s00216-025-06172-9","DOIUrl":"https://doi.org/10.1007/s00216-025-06172-9","url":null,"abstract":"<p><p>Deoxynivalenol (DON), a highly stable and globally prevalent mycotoxin, has become a critical food safety concern due to its widespread contamination in animal feed, particularly in corn, wheat, and other cereal-based ingredients. As one of the most frequently detected mycotoxins in feedstuffs, DON contamination not only causes significant economic losses in livestock production but also poses severe health risks to animals, including vomiting, immunosuppression, and growth retardation, which may ultimately affect human health through the food chain. Existing detection methods for DON are often limited by time-consuming procedures or analytical complexity. Here, we report a novel surface-enhanced Raman scattering-based lateral flow immunoassay (SERS-LFIA) for rapid, sensitive, and specific detection of DON residues in animal feeds. The biosensor employs core-shell Au@4-MBA@Ag nanoparticles functionalized with 4-mercaptobenzoic acid (4-MBA) as a Raman reporter and DON-specific antibodies for target recognition. After systematic optimization, the SERS-LFIA platform achieved both qualitative and quantitative detection within 16 min, with an exceptionally low limit of detection (LOD) of 0.01 µg/kg. The assay demonstrated excellent specificity, showing no cross-reactivity with other major mycotoxins, including aflatoxin B<sub>1</sub>, zearalenone, and ochratoxin A. Remarkable reproducibility was evidenced by intra- and inter-batch coefficients of variation (CV) of 3.51% and 2.19%, respectively. The test strips maintained stability for at least 3 months at 4 ± 0.5 °C and for 2 months at 25 ± 0.5 °C, making them particularly suitable for routine monitoring in feed mills and farms. This innovative SERS-LFIA system represents a significant advancement in mycotoxin detection technology, offering a robust, field-deployable solution for monitoring DON contamination in animal feed, which is crucial for ensuring feed safety and animal health.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145336251","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}
Vera M Scharek, Tommy Kröger, Karin Keil, Heike Traub, Björn Meermann
{"title":"A new elemental analytical approach for microplastic sum parameter analysis-ETV/ICP-MS with CO<sub>2</sub>.","authors":"Vera M Scharek, Tommy Kröger, Karin Keil, Heike Traub, Björn Meermann","doi":"10.1007/s00216-025-06146-x","DOIUrl":"https://doi.org/10.1007/s00216-025-06146-x","url":null,"abstract":"<p><p>Microplastics (MPs) are pervasive environmental pollutants and are considered one of the main challenges of our time. However, a fast and comprehensive analytical approach for MP analysis in complex matrices traceable to SI units is still lacking. In this context, we report a fast screening tool for the sum parameter analysis of MPs using electrothermal vaporization (ETV) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). In our proof-of-concept study, we observed size-independent detection of MPs as peaks above the <sup>13</sup>C<sup>+</sup> signal background in the nano- to micrometer range without limitations regarding the polymer type. Quantification of the <sup>13</sup>C<sup>+</sup> MP signals was accomplished via an external gas calibration utilizing dynamic dilution of carbon dioxide with argon, yielding recovery rates of 80-96% for MP reference material (RM) of polymer types commonly found in the environment. The applicability to a soil sample was demonstrated through spiking experiments with a polyethylene (PE) MP RM in soil. The limit of detection (LOD) was estimated to be 0.13 µg C, equaling the detection of a single spherical low-density-PE particle of about 70 µm, and a limit of quantification (LOQ) of 0.42 µg C.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145328003","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}
Candela Melendreras, Jesús Montero, José M Costa-Fernández, Ana Soldado
{"title":"Trends on vibrational spectroscopy tools in the agri-food sector.","authors":"Candela Melendreras, Jesús Montero, José M Costa-Fernández, Ana Soldado","doi":"10.1007/s00216-025-06166-7","DOIUrl":"https://doi.org/10.1007/s00216-025-06166-7","url":null,"abstract":"<p><p>Ensuring food safety and quality has become a critical priority in response to increasing global demand and regulatory requirements. To address these challenges, the food industry is demanding sensitive, selective, and robust analytical strategies. Among these, non-destructive spectroscopic sensors (NDSS), particularly those based on vibrational spectroscopy such as near infrared (NIR) and Raman spectroscopy, have demonstrated significant potential for rapid, in situ analysis of food matrices without compromising sample integrity. Current research efforts are focused on the miniaturization and cost-effective design of spectroscopic instrumentation, enabling the development of portable devices suitable for real-time food monitoring across the supply chain. In parallel, advanced chemometric techniques and machine learning algorithms are revolutionizing spectral data interpretation, enhancing model calibration, transferability, and predictive reliability. Artificial intelligence approaches in spectroscopic workflows facilitate the extraction of meaningful patterns from large and complex spectral datasets. Together, these advanced vibrational proposals are converging toward the realization of intelligent, real-time decision-making systems that support sustainable, efficient, and safe food production and distribution, redefining the standards of food quality control in modern agri-food systems.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145317950","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}
Ghulam Hussain Qasim, Lisa Harris, Vaughn Mangal, Mario Montesdeoca, Svetoslava Todorova, Charles Driscoll
{"title":"Ultra-high-resolution mass spectrometric analysis of mercury-DOM complexes extracted from lake water at ambient pH.","authors":"Ghulam Hussain Qasim, Lisa Harris, Vaughn Mangal, Mario Montesdeoca, Svetoslava Todorova, Charles Driscoll","doi":"10.1007/s00216-025-06122-5","DOIUrl":"https://doi.org/10.1007/s00216-025-06122-5","url":null,"abstract":"<p><p>Understanding the elemental and structural composition of mercury-dissolved organic matter (Hg-DOM) complexes is crucial for comprehending Hg speciation, bioavailability, and transformations in aquatic ecosystems. However, low concentrations of these organo-metal complexes in natural waters and extraction at acidic pH constrain their characterization. Here, we used solid phase extraction (SPE) methodology to extract Hg-DOM complexes at ambient pH and validated their preconcentration by preserving the composition for identification using ultra-high-resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS). While the dissolved organic carbon (DOC) extraction efficiency was higher with cartridges containing styrene divinylbenzene copolymer (PPL) than silica structure bonded with hydrocarbon chains (C18), Hg in both extracts showed no significant difference. FT-ICR-MS analysis revealed that Hg-DOM complexes extracted by C18 cartridges were aliphatic with smaller carbon chains (16-18), whereas complexes extracted with PPL exhibited both aliphatic and aromatic characteristics with a wide distribution of carbon chains ranging from 17 to 25. The C18 cartridge appeared to be selective in extracting and preserving the nonpolar complexes, as evidenced by the identification of two molecular formulae, C<sub>16</sub>H<sub>31</sub>HgNO<sub>3</sub> and C<sub>16</sub>H<sub>35</sub>HgNO<sub>2</sub>S, with m/z ratios of 487.2 and 507.21, across triplicate extractions. This study addresses the challenge of the spectroscopic limitation of Hg-DOM identification by extracting these complexes at circumneutral pH and presumably preserving them from dissociation during extraction.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145312088","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":"Recent applications of parylene and pyrolyzed parylene in sensors and devices: a review.","authors":"He Zhao, B Jill Venton","doi":"10.1007/s00216-025-06150-1","DOIUrl":"https://doi.org/10.1007/s00216-025-06150-1","url":null,"abstract":"<p><p>Parylene is an insulating polymer that is coated in thin layers on sensors and devices. It exhibits excellent gas and moisture impermeability, enabling it to function as a biocompatible encapsulation layer. Parylene is commonly deposited by chemical vapor deposition (CVD) on substrates, with coating thicknesses ranging from nanoscale to microscale, depending on the amount of precursor loaded into the parylene coater. Parylene was deposited on cell culture devices made from 3D printing resins, and it prevents leachates that are toxic to cells, enabling long-term cultures. Pristine parylene is also used for sealing implantable sensors, the cantilever of atomic force microscopy (AFM), and microelectromechanical systems (MEMS), preventing damage in harsh environments. In addition to the intrinsic insulating properties of parylene, parylene is pyrolyzed at high temperatures, inducing structural reformation and converting it to a conductive material. Pyrolyzed parylene is utilized for electrochemical sensing of molecules, coupled with cyclic voltammetry (CV), fast scan cyclic voltammetry (FSCV), or immunoassays. For example, pyrolyzed parylene sensors can be used for in vivo tracking of neurotransmitters. A CO<sub>2</sub> infrared laser can be an alternative method to induce the graphitization of parylene films. Laser-induced graphene (LIG) is used to fabricate microsupercapacitors. A plasma deposition method for parylene has recently been developed, enabling the creation of a crosslinked structure that favors the immobilization of antigens for immunoassay fabrication. Overall, parylene is easy to coat on a variety of materials and provides biocompatible insulation of analytical devices, with easy pyrolysis to carbon used in sensors.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145311914","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}
 Carapito, F Amaro, A Teixeira-Marques, R Henrique, C Jerónimo, A C A Roque, F Carvalho, J Pinto, P Guedes de Pinho
{"title":"Influence of pre-analytical factors and biological variability on the urinary volatilome.","authors":"Â Carapito, F Amaro, A Teixeira-Marques, R Henrique, C Jerónimo, A C A Roque, F Carvalho, J Pinto, P Guedes de Pinho","doi":"10.1007/s00216-025-06137-y","DOIUrl":"https://doi.org/10.1007/s00216-025-06137-y","url":null,"abstract":"<p><p>Volatile organic compounds (VOCs) in urine have shown increasing promise as non-invasive biomarkers for the early detection and monitoring of diseases. However, their volatile nature may make them highly susceptible to pre-analytical factors, presenting significant challenges for consistent biomarker discovery and reproducibility within metabolomic workflows. This study aimed to assess the impact of four critical pre-analytical variables, including fasting state, centrifugation procedures, room temperature (RT) stability, and freeze-thaw (FT) cycles, as well as intra- and inter-individual variability on the profiles of urinary VOC in general and volatile carbonyl compounds (VCC), in particular. Urine samples were analysed using headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME/GC-MS). Our findings demonstrate that, although multivariate analysis did not discriminate between fasting and non-fasting states, univariate analysis revealed that the levels of distinct VOCs and VCCs significantly differed between both states. The urinary VOC or VCC profiles were very similar under both standard centrifugation and sequential mild pre-centrifugation followed by ultracentrifugation. These findings suggest that supernatants obtained from assays involving ultracentrifugation are suitable for volatilome analysis. RT stability studies demonstrated that VOC profiles remain stable for up to 21 h at RT, whereas VCC profiles showed alterations after 14 h. Compound-specific variations were also observed following repeated FT cycles, with several VOCs disclosing significant changes after two cycles, while VCC profiles remained stable, with no significant alterations detected. Both intra- and inter-individual variability were high, as evidenced by relative standard deviations exceeding 30% for most compounds and intraclass correlation coefficients below 0.4, indicating limited temporal reliability over a 2.5-month period with eight timepoint collections. These findings underscore the essential role of pre-analytical standardization in urinary volatile analysis and support the implementation of rigorous protocols to enhance data reproducibility and biomarker discovery in metabolomics.</p>","PeriodicalId":462,"journal":{"name":"Analytical and Bioanalytical Chemistry","volume":" ","pages":""},"PeriodicalIF":3.8,"publicationDate":"2025-10-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145297995","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}