bims-metlip Biomed News
on Methods and protocols in metabolomics and lipidomics
Issue of 2025–10–26
thirty papers selected by
Sofia Costa, Matterworks



  1. Clin Chem Lab Med. 2025 Oct 20.
       OBJECTIVES: Precise and accurate determination of urinary cortisol is important for diagnosis and monitoring of cortisol excess and deficiency. To achieve this, a selective and specific, isotope-dilution two-dimensional heart-cut liquid chromatography-tandem mass spectrometry (LC-MS/MS)-based method was developed.
    METHODS: A novel, two-dimensional heart-cut LC-MS/MS method was developed using a Waters Acquity BEH C18 column and a Raptor Biphenyl column, with water (A1) and with 0.2 mM ammonium fluoride in water (A2) and methanol (B1+B2) as mobile phases. This approach was complemented by a supported liquid extraction (SLE) sample preparation protocol. Matrix effects were assessed through post-column infusion experiments and comparisons of standard line slopes across matrices. A multi-day validation study evaluated accuracy and precision of the candidate reference measurement procedure (RMP) and measurement uncertainty (MU) was estimated in compliance with current guidelines. Reproducibility was assessed by performing a method comparison study between two independent laboratories.
    RESULTS: In the first LC column dimension, cortisol and prednisolone were separated from cortisone, prednisone, and 20-beta-dihydrocortisone. Baseline separation of cortisol from prednisolone was achieved in the second dimension. No interfering signals were detected at the retention time for quantifier and internal standard transitions in any urine samples analysed. No significant matrix effect, ion suppression, or enhancement was observed. Linearity was successfully demonstrated (r≥0.999); residuals were randomly distributed in a quadratic model via linear regression with an 1/x weighting. The lower limit of the measuring interval was determined at 2.00 ng/mL (5.52 nmol/L), displaying a relative deviation of -0.1 %, a coefficient of variation (CV) of 2.9 %, and recoveries of 96-103 %. Intermediate precision ranged from 1.9-3.2 % and repeatability CV from 1.6-2.7 %. Relative mean bias ranged from -3.5-1.2 %, indicating method accuracy was unaffected by matrix variance. Measurement uncertainties (k=1) for cortisol were ≤3.4 % across different concentrations and sample types. The expanded uncertainty at a 95 % confidence level (k=2) was ≤6.8 %. An increased number of measurements (n=6) for target value assignment reduced the uncertainty to 0.8-1.3 % (k=1), yielding an expanded uncertainty (k=2) of 1.7-2.5 %.
    CONCLUSIONS: The validation results confirm the robustness, accuracy, and reliability of this RMP for determination of cortisol in human urine within a working range of 2.00-220 ng/mL (5.52-552 nmol/L).
    Keywords:  SI units; cortisol in urine; isotope dilution-liquid chromatography-tandem mass spectrometry; qNMR characterization; reference measurement procedure; traceability
    DOI:  https://doi.org/10.1515/cclm-2025-0522
  2. Metabolomics. 2025 Oct 18. 21(6): 151
       INTRODUCTION: The identification of unknown metabolites remains a major challenge in untargeted metabolomics using liquid chromatography-mass spectrometry (LC-MS). This process typically depends on comparing mass spectral or chromatographic data to reference databases or deciphering complex fragmentation in tandem mass spectra. While current machine learning methods can predict metabolite structures using MS/MS (MS2) data, no approaches, to our knowledge, use only mass-to-charge ratio (m/z) and retention time (RT) from LC-MS data.
    OBJECTIVE: To explore the potential of using the mass-to-charge ratio (m/z) and retention time (RT) from LC-MS data as standalone predictors for metabolite classification and propose a modeling framework which can be implemented internally on standalone datasets.
    METHODS: We trained machine learning models on 20 mouse lung adenocarcinoma tumor samples with 7,353 features and validated them on a dataset of 81 samples with 22,000 features. A total of 120 combination of preprocessors and models were assessed. Features were classified as "lipid" or "non-lipid" based on the Human Metabolome Database (HMDB) taxonomy, and model performance was assessed using accuracy, area under the receiver operating characteristic curve (AUC), and area under the precision-recall curve (PR). We replicate the process in an independent dataset generated using human plasma samples.
    RESULTS: We classified untargeted LC-MS features as "lipid" or "non-lipid" per the HMDB super class taxonomy and evaluated model performance. A framework including steps to choose the preprocessors and models for metabolite classification was designed. In our lab, tree-based models demonstrated superior performance across all metrics, achieving high accuracy, AUC, and PR which was consistent with the independent dataset.
    CONCLUSION: Our results demonstrate that metabolites can be classified as "lipid", "non-lipid" using only m/z and RT from untargeted LC-MS data, without requiring MS2 spectra. Although this study focused on lipid classification, the approach shows potential for broader application, which warrants further investigation across diverse compound classes, detection methods, and chromatographic conditions.
    Keywords:  LC–MS; Machine learning; Mass–to–charge ratio; Retention time; Unknown metabolites
    DOI:  https://doi.org/10.1007/s11306-025-02343-y
  3. Anal Chim Acta. 2025 Dec 08. pii: S0003-2670(25)01046-3. [Epub ahead of print]1378 344652
       BACKGROUND: 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.
    RESULTS: 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.
    SIGNIFICANCE: 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.
    Keywords:  Lipidomics; Liquid chromatography; Mass spectrometry; Sample normalization; UV–Visible spectrometry
    DOI:  https://doi.org/10.1016/j.aca.2025.344652
  4. Drug Metab Bioanal Lett. 2025 ;18(1): 71-81
       OBJECTIVE: A unique liquid chromatography-tendon mass spectrometric technique for the determination of metformin and vildagliptin in K3EDTA human plasma was developed and verified as per the USFDA guidelines of bioanalysis.
    METHODS: The chromatographic separation was achieved using a Cosmosil CN (150 x 4.6 mm, 5 μm) column with an isocratic elution pattern using 10 mM ammonium formate (pH 5.0) and methanol in the ratio of 30:70 v/v as a mobile phase. A mass spectrometer coupled with an electrospray ionization (ESI) source operating in the positive ion was used for detection. Data were obtained in the multi-reaction monitoring (MRM) acquisition mode. Metformin D6 and vildagliptin D7 were used as internal standards, with the flow rate at 1.0 mL/min throughout the experiment. The drugs were extracted by solid phase extraction (SPE) packed with Phenomenex Strata-X. Extraction of the drug was achieved using methanol: 5 mM sodium lauryl sulphate solvent mixture in equal proportions.
    RESULTS: The retention time for MET and VLG were 3.2 and 3.8 minutes individually. The drugs were extracted by SPE with good recovery of 89.44% and 87.57% for metformin and ISTD and 92.26% and 89.58% for vildagliptin and ISTD, respectively. Sample elution was performed using solid phase extraction (SPE), and this technique produced very pure extracts with good recovery rates. A liner calibration curve was found in the range of 0.5-400 ng/mL for MET and 0.2-160 ng/mL for VLG with a correlation coefficient r2 > 0.99.
    CONCLUSION: The aforementioned technique is reliable and effective for monitoring bioequivalence investigations in human participants.
    Keywords:  Bioanalysis; LC-MS/MS; metformin; multi-reaction monitoring.; solid phase extraction; vildagliptin
    DOI:  https://doi.org/10.2174/0118723128357810250304055648
  5. ACS Meas Sci Au. 2025 Oct 15. 5(5): 751-759
      Human milk oligosaccharides (HMOs) are a biologically important class of carbohydrates responsible for promoting the healthy development of infants. However, to better understand their specific biological roles, analytical techniques are needed to unambiguously characterize them. While liquid chromatography-tandem mass spectrometry (LC-MS/MS) remains the gold standard for HMO analysis, new orthogonal techniques are desired for improving their isomer analysis. Ion mobility spectrometry-mass spectrometry (IMS-MS) has emerged as a complementary technique to LC-MS/MS but has seen little use toward HMO sequencing analysis beyond the construction of collision cross section (CCS) databases. In this work, we describe the use of collision-induced dissociation performed prior to high-resolution cyclic ion mobility separations (i.e., pre-cIMS CID) in conjunction with CCS measurements to characterize the linkage positioning in various HMOs irrespective of the starting precursor ion. We then demonstrated how our developed approach could be used to sequence an unknown HMO present in a purified extract. Lastly, we applied our workflow to sequence an isomeric mixture in the same extract using cIMS/cIMS instead of pre-cIMS CID. Overall, our developed approach is a first step toward standard-free de novo HMO sequencing as well as being a complementary and orthogonal method to existing LC-MS/MS-based workflows.
    Keywords:  carbohydrates; human milk oligosaccharides; ion mobility spectrometry; mass spectrometry; separation science; sequencing
    DOI:  https://doi.org/10.1021/acsmeasuresciau.5c00083
  6. Anal Chim Acta. 2025 Dec 08. pii: S0003-2670(25)01045-1. [Epub ahead of print]1378 344651
       BACKGROUND: Carboxylic acids are vital metabolites widely present in living organisms, playing critical roles in various biological processes. Alterations in carboxylic acid profiles are often associated with inborn errors of metabolism (IEMs), which can lead to severe consequences or even mortality without timely treatment. Monitoring these metabolites through time-series analysis is essential for understanding disease progression. However, achieving high-throughput analysis of carboxylic acids using conventional chromatographic techniques remains a significant challenge.
    RESULTS: This study introduces a 5-channel multiplex method using liquid chromatography‒electrospray ionization‒tandem mass spectrometry (LC‒ESI‒MS/MS) to quantify essential carboxylic acids in urine. The method employs butanol isotopes to form butyl derivatives (D0-, D3-, D5-, D7-, and D9-carboxylic acid butyl ester). Validation results demonstrated high accuracy (85.22 %-115.16 %) for mixture estimation, with analyte quantification accuracies ranging from 79.1 % to 116.6 % and precisions below 15 % for most compounds. The validated method was applied to four urine samples in a simulated time-series study, highlighting its effectiveness in tracking metabolic changes.
    SIGNIFICANCE: The innovative multiplex strategy significantly enhances the throughput and precision of carboxylic acid quantification. By enabling efficient time-series analyses, this approach contributes to the study of IEMs and accelerates clinical diagnostics, offering promising applications in both research and healthcare.
    Keywords:  Carboxylic acid; Chemical isotope labeling; Inborn error metabolism; LC-MS/MS; Multiplex analysis
    DOI:  https://doi.org/10.1016/j.aca.2025.344651
  7. Ann Lab Med. 2025 Oct 23.
       Background: Alpha-fetoprotein (AFP) and its isoform AFP-L3 are well-established serum biomarkers for hepatocellular carcinoma (HCC), a common malignancy and a leading cause of cancer-related mortality worldwide. Current methods for measuring these biomarkers are primarily lectin-based assays including the liquid-phase binding assay (LiBA) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), both of which have limitations in diagnostic sensitivity and clinical utility for samples with low AFP concentrations. We aimed to develop a lectin-independent LC-MS/MS method for quantifying fucosylated AFP proteins (AFP-Fuc%).
    Methods: We conducted analytical validation, including method comparisons, over 2 months. The analytical sensitivity and diagnostic performance of this method were evaluated using 525 human serum samples-235 from HCC patients and 290 from non-HCC individuals-and compared with those of LiBA, which measured AFP-L3 levels.
    Results: The LC-MS/MS method demonstrated acceptable within-laboratory imprecision (CVs<17.1%) without detectable bias, carryover, or matrix effects. Our method exhibited a broader linear dynamic range (spanning five orders of magnitude) and 10-fold higher analytical sensitivity than LiBA. The diagnostic performance of our method was significantly superior to that of LiBA, particularly in patients with low AFP concentrations (<7 ng/mL, P <0.001), with improved accuracy, sensitivity, and precision at a specificity of 96.2%.
    Conclusions: The validated LC-MS/MS method demonstrated robust analytical performance and superior diagnostic accuracy over LiBA for HCC diagnosis while avoiding the inherent limitations of lectin-based assays. Our LC-MS/MS assay shows promise for early HCC detection and may contribute to enhanced patient care.
    Keywords:  Alpha-fetoprotein; Automation; Fucosylation; Glycopeptide; Hepatocellular carcinoma; Liquid Chromatography; Mass spectrometry
    DOI:  https://doi.org/10.3343/alm.2025.0003
  8. Biomed Chromatogr. 2025 Dec;39(12): e70242
      Several studies have reported detection methods for etomidate and its analogues, metomidate and propoxate, but data on their pharmacokinetics and bioavailability are limited. This study develops a UPLC-MS/MS method to simultaneously detect these compounds and evaluates their pharmacokinetics and bioavailability in mice. Plasma samples were processed using methanol-induced protein precipitation. The separation was conducted on a UPLC BEH C18 column with an acetonitrile-water (containing 0.1% formic acid) as mobile phase at a flow rate of 0.4 mL/min, achieving elution within 4 min. Quantitative analysis was performed using MRM mode coupled with ESI in positive ion mode. In this study, mice received etomidate, metomidate, and propoxate via intravenous (1 mg/kg) and oral (10 mg/kg) routes, and the pharmacokinetics were evaluated. The calibration curves demonstrated excellent linearity within the ranges of 0.5-1000 ng/mL for etomidate, 0.504-1080 ng/mL for metomidate, and 0.77-1540 ng/mL for propoxate in mouse plasma, with correlation coefficients (r values) exceeding 0.998. The developed UPLC-MS/MS method was successfully utilized to analyze the pharmacokinetics of etomidate, metomidate, and propoxate. The absolute bioavailability of etomidate, metomidate, and propoxate was determined to be 14.0%, 21.3%, and 15.3%, respectively.
    Keywords:  UPLC‐MS/MS; etomidate; metomidate; pharmacokinetics; propoxate
    DOI:  https://doi.org/10.1002/bmc.70242
  9. J Chromatogr A. 2025 Oct 16. pii: S0021-9673(25)00812-X. [Epub ahead of print]1764 466468
      An automated magnetic solid-phase extraction (MSPE) method was developed for the simultaneous enrichment and quantification of eight catecholamines and their metabolites in human urine. This method utilized carboxyl- and secondary amine-functionalized poly (polystyrene-co-divinylbenzene-co-N-vinylpyrrolidone) coated silica magnetic beads, combined with ID-LC-MS/MS. Through systematic optimization, the automated MSPE process efficiently extracted the target analytes from urine within 10 min. The validated method demonstrated excellent sensitivity and linearity over a range of 500-fold (with R2 > 0.995 for all analytes), along with outstanding accuracy (recoveries of 95.22 % -104.07 %) and precision (RSD <10 %). No significant matrix effects or interference were observed. The method was successfully applied to analyze the samples from the 2024 National External Quality Assessment Program for Catecholamines and Their Metabolites (batches 202,411 and 202,412), where deviations for the eight analytes at two different concentrations ranged from -8.31 % to 10.43 %, confirming high accuracy and reliability. Furthermore, an inter-laboratory comparison showed a strong correlation between the results from our system and the established reference values, underscoring the method's consistency and reproducibility. Given its robustness and efficiency, this automated MSPE-ID-LC-MS/MS method serves as a valuable tool for diagnosing catecholamine-secreting tumors and contributes to the advancement of precision medicine and laboratory automation.
    Keywords:  Catecholamines and their metabolites; ID-LC-MS/MS; Magnetic solid-phase extraction; Method validation
    DOI:  https://doi.org/10.1016/j.chroma.2025.466468
  10. Anal Chim Acta. 2025 Dec 08. pii: S0003-2670(25)01092-X. [Epub ahead of print]1378 344698
       BACKGROUND: Triacylglycerols (TGs) are the most abundant lipids in the human body and the primary source of energy storage. TGs are comprised of three fatty acyls with various lengths and double bond composition, complicating structural annotation when performing lipidomics by LCMS. Data-independent acquisition (DIA) based lipidomics enables a continuous and unbiased acquisition of all TGs, creating the potential for more comprehensive TG analysis. However, TG identification in DIA lipidomics data is challenging due to the difficulty analyzing multiplexed tandem mass spectra (MS2).
    RESULTS: In this study, we present DIATAGeR, an R package aimed to improve and automate TG identifications to the molecular species level in DIA-based lipidomics. With DIATAGeR, TGs are identified using a TG-centric approach, where each TG in the reference database is considered as an analysis target, searched in DIA spectra, and scored using a logistic regression machine learning algorithm. Additionally, DIATAGeR uses a false discovery rate (FDR) correction calculated by a target-decoy approach to improve the confidence of TG identification and limit false positives due to interference from unrelated ions. The performance of DIATAGeR was validated in a lipidomic study of liver and plasma samples from mice with metabolic dysfunction-associated steatohepatitis (MASH) and healthy controls. All 9 TG standards were annotated at an FDR <0.1 in both datasets. When benchmarked against MS-DIAL, TGs identified by DIATAGeR contained 18 % and 12 % more even-carbon fatty acyls in liver and plasma datasets, respectively.
    SIGNIFICANCE: DIATAGeR is a valuable tool for streamlining complex TG annotation in DIA-lipidomics data. It supports vendor-neutral MS spectra data formats and offers a customizable reference database. By combining TG-centric and target-decoy approaches, DIATAGeR showed improvements in TG identification by addressing primary challenges associated with multiplexed MS2 spectra. DIATAGeR is freely available at https://github.com/Velenosi-Lab/DIATAGeR.
    Keywords:  Data-independent acquisition; Lipidomics; Machine learning; Mass spectrometry; R package; Triacylglycerol annotation
    DOI:  https://doi.org/10.1016/j.aca.2025.344698
  11. J Pharm Biomed Anal. 2025 Oct 17. pii: S0731-7085(25)00543-6. [Epub ahead of print]268 117202
      Targeted metabolomics focuses on the quantification of a selected set of metabolites of interest from biological samples. The obtained data is used to better understand the physiological and pathophysiological state of an organism. Plasma samples are commonly analyzed with liquid chromatography coupled to mass spectrometry but require prior sample preparation. In preclinical studies sample volumes are often limited and metabolites of interest are typically present at low concentrations. As a result, there is a growing need for miniaturized sample preparation methods with high extraction efficiency. This review discusses key aspects in sample preparation highlighting the limitations associated with the more conventional methods, such as limited sample clean-up, low selectivity, long extraction times, limited extraction efficiency and the use of hazardous or toxic organic solvents. To address their challenges, novel sample preparation strategies have been developed. Examples that will be discussed are solid phase microextraction, microextraction by packed sorbents, 3D-printed sorbents, molecularly imprinted polymers, magnetic nanoparticles, magnetic ionic liquid-based liquid-liquid microextraction, dispersive liquid-liquid microextraction, nanoconfined liquid phase nanoextraction and supported liquid membrane-electromembrane extraction. A critical evaluation of these sample preparation methods is presented in the context of targeted metabolomics. Furthermore, inspiration is found in untargeted metabolomics and other bioanalytical applications for alternative sample preparation methods that may hold potential for plasma in targeted metabolomics.
    Keywords:  Liquid Chromatography – Mass Spectrometry; Microextraction; Plasma; Sample preparation; Targeted metabolomics
    DOI:  https://doi.org/10.1016/j.jpba.2025.117202
  12. Front Chem. 2025 ;13 1631203
      An accurate, reliable, and sensitive method was successfully developed to simultaneously determine p-Nitroaniline (p-NA) and its metabolites in blood based on the hyphenated technology of quadrupole-orbitrap high resolution mass spectrometry (Q-Orbitrap HRMS) and ultra-performance liquid chromatography (UPLC). After the blood sample was extracted with ethyl acetate, the organic layer was taken for injection and analysis. Within the concentration range of 1-100 μg/L, the calibration curves of p-NA and its metabolites had a good linearity, with correlation coefficient(r) values greater than 0.999. This method has excellent precision and accuracy. The intra- and inter-day coefficients of variation (CVs) were less than 9.9% and 8.7% respectively, and the analytical accuracy ranged from 83.1% to 101.3%. The lower limits of detection (LLODs) for all target analytes were between 0.6 μg/L and 2.2 μg/L, and the lower limits of quantification (LLOQs) were between 2.0 μg/L and 7.4 μg/L. In addition, the application potential of this method was verified by analyzing the blood samples of workers exposed to p-NA. The results indicated that this method was accurate, reliable and sensitive, and was applicable to the detection of p-NA and its metabolites in the blood.
    Keywords:  UPLC-Q-Orbitrap HRMS; blood; metabolite; occupational exposure; p-Nitroaniline
    DOI:  https://doi.org/10.3389/fchem.2025.1631203
  13. Front Cell Infect Microbiol. 2025 ;15 1658802
       Introduction: Over the last two decades, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) has been introduced into the routine diagnostic practice of microbiological laboratories for the rapid taxonomic identification of bacteria and yeasts. However, a method that effectively identifies microbes directly from clinical samples using MALDI-TOF MS has not yet been found. One of the promising targets is microbial polysaccharides, which are abundant structures in bacterial and fungal cells. Their rapid and inexpensive analysis, nevertheless, is complicated. This study focused on detecting microbial polysaccharides, such as lipopolysaccharides, using MALDI-TOF MS and liquid chromatography-tandem mass spectrometry (LC-MS). We developed a method for fingerprinting polysaccharides by acid hydrolysis and enzymatic digestion.
    Methods: The mono- and oligosaccharides are then derivatized with a newly designed probe (vanillyl pararosaniline, the HD ligand), enabling efficient ionization without the use of the MALDI matrix. For precise analysis of polysaccharides, the hydroxyl groups can be esterified by formic acid.
    Results: The method was validated using several saccharides as well as Escherichia coli lipopolysaccharides (O26:B6, O55:B5, and O111:B4). Derivatization using the HD ligand also allows the detection of structures containing amines and phosphate groups in positive ion mode. We optimized the method using crude bacteria (Escherichia coli, Salmonella enterica, Shigella dysenteriae, Shigella boydii, Shigella flexneri, and Legionella pneumophila, Staphylococcus aureus) and yeasts (Candida albicans, C. kudriavzevii, and C. tropicalis).
    Discussion: This approach opens the possibility of directly detecting microbial polysaccharides from clinical specimens. Laser Desorption/Ionization Time-of-Flight Mass Spectrometry (LDI-TOF MS) using a specific self-ionizable ligand enables direct ionization without the need for an additional matrix, allowing for the particular detection of molecules of interest while suppressing the background signal.
    Keywords:  LC-MS; MALDI-TOF MS; bacteria; mass spectrometry; microbiology; polysaccharide
    DOI:  https://doi.org/10.3389/fcimb.2025.1658802
  14. Anal Chem. 2025 Oct 19.
      LC-MS-based nontargeted analysis is essential for identifying key chemicals in real-world samples. A significant technical bottleneck, however, arises in resolving the structures of unknown chemicals from their mass spectra. This challenge is exacerbated by the limited information available in existing databases and the poor quality of the acquired mass spectra. To address these issues, we developed the Fragmental Chain Characterization (FCC) method, which assigns formulas to unknown compounds based on their mass spectra. When integrated with the Chromatographic Retention Behavior (CRB) approach, the CRB-FCC method enables the identification of the same compound across different samples, leveraging consistent retention times and assigned formulas, even when sampling conditions cause significant variations in mass spectra. The CRB-FCC method is validated using a large set of 1,475 chemical standards. In comparison to conventional annotation methods, which rely on mass spectral matching, CRB-FCC has shown the ability to accurately annotate compounds even when their mass spectra are of poor quality or absent from the database. As a case in point, we combined CRB-FCC and NMR characterization to successfully identify unknown yellow-hue impurities in biosynthesized plastics sourced from local industrial sources, addressing a key barrier to their practical applications. We anticipate that CRB-FCC, a standardized protocol for data acquisition and interpretation in nontargeted analysis, will accelerate its adoption across both academia and industry.
    DOI:  https://doi.org/10.1021/acs.analchem.5c03451
  15. J Chromatogr A. 2025 Oct 11. pii: S0021-9673(25)00803-9. [Epub ahead of print]1764 466459
      Non-target screening (NTS) of plant secondary metabolites is analytically challenging due to the complexity of mixtures with structurally similar compounds and isomers. This study evaluates the added value of ion mobility spectrometry (IMS) and comprehensive two-dimensional liquid chromatography (LC × LC) for enhancing separation, mass spectral quality, chromatographic structure and from access to collisional cross section (CCS) values in NTS workflows. Four LCHRMS configurations were compared: RPLCHRMS, HILICHRMS, RPLC × HILICHRMS, and HILIC × RPLCHRMS, each with and without travelling wave (TW)IMS. Data were acquired in data-independent acquisition (DIA) mode. Phenolic compounds in wheat flag leaf extracts were analyzed as a representative case. The results show that mass spectral purity improved up to 74 times when hyphenating RPLC with IMS for peaks with intensities <1.5 × 104. The compound groups: flavones, flavan-3-ols, benzoic acid derivatives and phenolic acids were separated into distinct retention time regions in RPLC × HILIC, while co-eluting in RPLC and HILIC. Only two of ten isomeric pairs were partially resolved by IMS, with resolutions of 0.50 and 0.63, whereas RPLC achieved resolution values of 29 and 13 for the same pairs. Notably, the only isomers with IMS resolution ≥ 0.5 had m/z > 447. We showed that large [Formula: see text] deviations (-9.47 %) were observed when several deprotomers of a molecule were created and separated in IMS. Deprotomers are not accommodated for in the machine learning prediction models, which limits their use for such molecules. The complementary strengths of IMS and LC × LC should be exploited strategically to address specific analytical goals in plant metabolite screening.
    Keywords:  2D-LC; Ion mobility; Mass spectral quality; Structured chromatogram
    DOI:  https://doi.org/10.1016/j.chroma.2025.466459
  16. Analyst. 2025 Oct 22.
      Electron-induced dissociation methods, particularly electron impact excitation of ions from organics (EIEIO), offer enhanced capabilities for lipid structural elucidation over traditional collision-induced dissociation (CID). Despite their analytical promise, the practicality of EIEIO within routine liquid chromatography-mass spectrometry (LC-MS) workflows remains largely unexplored. In this study, we optimised LC-EIEIO-MS analysis for the rapid and detailed structural annotation of glycerides and phospholipids. We evaluated the effects of reaction times, accumulation times, and electron kinetic energies using lipid standards from multiple classes and at varying concentrations. Our results revealed that short reaction times of 30 ms consistently yielded stronger diagnostic signals crucial for lipid class identification and sn-position discrimination at concentrations as low as 200 pg on column. To systematically infer the position of double bonds from EIEIO spectra, we introduced LipidOracle, a software that tests all possible isomers and correctly accounts for missing data, noise, and crowded spectra. We demonstrated that longer accumulation times of 200 ms were most effective for determining carbon-carbon double bond (CC) positions, particularly in polyunsaturated lipids. Finally, we evaluated the performance of EIEIO with liver and plasma extracts. Overall, we demonstrate that comprehensive lipid structural characterisation, including sn-position and double bond locations in fatty acyl chains, is achievable within typical LC-MS timescales (∼0.2 s). Our findings outline practical guidelines for high-throughput analysis of complex lipid samples by EIEIO.
    DOI:  https://doi.org/10.1039/d5an00567a
  17. Environ Sci Technol. 2025 Oct 22.
      The human exposome features a highly expansive chemical space and substantial individual variability. Although screenings of xenobiotic compounds have revealed exposure landscapes of specific compounds, significant bottlenecks remain in profiling their biotransformed products for comprehensive exposome-wide analysis, including limitations to known metabolites, challenges in new metabolite annotation, and low throughput. In this study, we developed an untargeted metabolomics-based compound metabolite discovery network (CMDN) to facilitate high-throughput annotation of xenobiotic metabolites. CMDN integrates a triple-layered architecture comprising a differential expression metabolic space, a rule-based pseudo-MS1 candidature space and an MS2 spectrum similarity network. The utilities and advantages are demonstrated using pesticides as a representative example, given their widespread human exposure and well-documented toxicity. Coupled with enzymatic biotransformation assays involving 1,021 pesticides, CMDN nonredundantly annotated 2,886 biotransformed derivatives. Following multichannel validation, including standard verification, retention time prediction, murine studies, and time-course logistic modeling, identified metabolites were screened in a human cohort, revealing a novel, diverse, and extensive exposure spectrum. Collectively, this study establishes, for the first time, a scalable workflow for the annotation and screening of previously undercharacterized xenobiotic metabolites with unprecedented throughput, representing a significant advancement toward the characterization, interpretation, and prioritization of the human exposome.
    Keywords:  biotransformation; exposome; mass spectrometry; pesticides; rule-based annotation; unknown identification; untargeted metabolomic; xenobiotic metabolism
    DOI:  https://doi.org/10.1021/acs.est.5c08558
  18. Anal Chem. 2025 Oct 23.
      Amino acids (AAs) are closely linked to various diseases. Investigating their spatial distribution and content differences can provide deeper insights into specific disease mechanisms. Matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI) enables spatial visualization of biomolecules, but conventional matrices introduce significant background interference that limits the detection of small molecules such as AAs. On-tissue chemical derivatization (OTCD) using permanently charged pyridinium probes significantly enhances the detection sensitivity of poorly ionizable compounds like AAs, allowing for their spatial mapping. However, current quantitative mass spectrometry imaging (QMSI) strategies for AAs using conventional matrix remain limited, highlighting the urgent need for the development of a widely applicable absolute quantification method for AAs that integrates OTCD. In this study, a series of pyridinium salt-based MALDI-MS probes were designed and characterized, leading to the identification of an efficient candidate, 1-(4-(((2,5-dioxopyrrolidin-1-yl)oxy)carbonyl)-2-methylphenyl)-2,4,6-triphenylpyridin-1-ium tetrafluoroborate (DCMT-4FB). This probe was then combined with deuterium-labeled internal standard to establish calibration curve, and its linear correction capability was validated, demonstrating strong correlation coefficients. Furthermore, a novel quantitative endogenous substance spraying approach was employed to perform absolute quantification MSI analysis of AAs (leucine and isoleucine) in different regions of human hepatocellular carcinoma (HCC) tissue sections. Finally, by cospraying the DCMT-4FB probe with its deuterium-labeled isotope analog, DCMT-d2-4FB, the spatial distribution of AAs and other metabolites within HCC tissues was rapidly obtained, providing valuable insights for clinical research. This study highlights the superior AAs quantification capability of the DCMT-4FB probe and offers new perspectives for probe development and quantitative analysis of endogenous metabolites.
    DOI:  https://doi.org/10.1021/acs.analchem.5c01847
  19. J Chromatogr B Analyt Technol Biomed Life Sci. 2025 Oct 22. pii: S1570-0232(25)00386-1. [Epub ahead of print]1267 124832
      The ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) technique was utilized to detect rubusoside in mouse plasma and evaluate its pharmacokinetic behavior following oral administration at doses of 10 mg/kg and 20 mg/kg, as well as intravenous administration at 10 mg/kg. Plasma samples were prepared using a protein precipitation method employing acetonitrile as the precipitating agent and isoscoparin as the internal standard (IS). Chromatographic separation was performed on a UPLC high strength silica (HSS) T3 column under gradient elution conditions, using acetonitrile and 0.1 % formic acid in water as the mobile phase system. The calibration curve for rubusoside demonstrated excellent linearity across a concentration range of 3.5 to 1120 ng/mL. Both intra-day and inter-day precision values remained below 7 %, with accuracy ranging from 92.3 % to 108.1 %. Matrix effects were consistently within the range of 107.1 % to 110.0 %, and the recovery rate exceeded 74.2 %. Following oral administration, the absolute bioavailability of rubusoside was determined to be 1.00 % and 0.98 % at doses of 10 mg/kg and 20 mg/kg, respectively. These findings confirm that the developed UPLC-MS/MS method effectively supports the pharmacokinetic evaluation of rubusoside.
    Keywords:  Bioavailability; Pharmacokinetics; Rubusoside; UPLC-MS/MS
    DOI:  https://doi.org/10.1016/j.jchromb.2025.124832
  20. J Am Soc Mass Spectrom. 2025 Oct 19.
      We present a novel approach for achieving ultrahigh-resolution ion mobility (UHRIM) separations using a structures for lossless ion manipulation (SLIM) ion mobility-mass spectrometry (IM-MS) system. By incorporating a rounded-turn ion path design, ions can be transmitted and separated bidirectionally, enabling an iterative workflow in which mobility-separated ions are returned to the entrance of the serpentine path while preserving their separation order and position. This "iterative SLIM" (itSLIM) process can be repeated multiple times with little to no target ion loss to increase the effective path length of the mobility separation. As IM resolution scales with the square root of the separation path length, this method enhances IM resolution without increasing the form factor of the mobility device. It is particularly beneficial for targeted mobility analysis and confident identification where high specificity is required. UHRIM separation was achieved with a two-peak resolution of 2.48 for 18:1 Δ9-cis- and Δ9-trans-phosphatidylethanolamine (PE) lipid isomers at a path length of 120 m. By combining itSLIM separation over a 90-m path with MS/MS fragmentation analysis, a liquid chromatography (LC)-free workflow capable of definitive identification of the isomeric small molecule drugs norcodeine and norhydrocodone was achieved. The UHRIM separation simplifies the resulting MS/MS spectra and improves identification accuracy. Such capabilities are anticipated to enhance the throughput by reducing or eliminating LC run times and robustness of screening workflows. Iterative SLIM provides a powerful strategy for enhancing IM resolution, offering broad utility for high-performance analytical separations.
    DOI:  https://doi.org/10.1021/jasms.5c00282
  21. Biomed Chromatogr. 2025 Dec;39(12): e70238
      A robust and sensitive reversed-phase HPLC method was developed and validated for the quantitative determination of 3-methyl benzyl chloride, a potential genotoxic process impurity, in Meclizine HCl formulations. The separation was achieved on a C18 column using an isocratic mobile phase consisting of a 0.025-M sodium 1-heptanesulfonate buffer (pH 4.0, adjusted with 0.1 N sulfuric acid) and acetonitrile (600:400, v/v). Detection was performed at 210 nm. A quality-by-design approach, specifically a Box-Behnken design, was employed to optimize key chromatographic parameters including flow rate, acetonitrile concentration, and column temperature. The impact of these critical method variables was evaluated on retention time, tailing factor, and theoretical plate count to ensure method robustness and optimal performance. The method was validated per ICH guidelines, assessing specificity, linearity, accuracy, precision, robustness, and limits of detection (LOD) and quantification (LOQ). The LOD and LOQ were determined to be 0.016% and 0.048%, respectively, allowing for trace-level detection of 3-methyl benzyl chloride. The method demonstrated excellent specificity, sensitivity, accuracy (recoveries 95.1%-102.1%), and precision (RSD ≤ 10.0%). This validated and QbD-optimized method is suitable for routine quality control analysis in pharmaceutical manufacturing, ensuring the safety and regulatory compliance of Meclizine HCl formulations.
    Keywords:  3‐methyl benzyl chloride; HPLC; impurity profiling; meclizine HCl; method development; validation
    DOI:  https://doi.org/10.1002/bmc.70238
  22. J Vis Exp. 2025 Oct 03.
      This study systematically evaluates the comparative performance of two mass spectrometry acquisition modes, data-dependent acquisition (DDA) and data-independent acquisition (DIA), coupled with ultra-high-performance liquid chromatography-quadrupole-orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap HRMS) for comprehensive chemical profiling of complex traditional Chinese medicine (TCM) formulations. Huaihua Powder, a classical formulated prescription, was employed as a model system for empirical assessment. Optimized DDA and DIA acquisition methods were separately established: the DDA method incorporated a targeted precursor ion selection strategy with customized fragmentation parameters, while the DIA method employed a segmented variable window strategy to cover the target m/z range, performing unbiased fragmentation on all precursor ions. Compound identification was executed using Compound Discoverer software. The comparative evaluation specifically focused on the performance characteristics of the two acquisition modes, encompassing the number of identified compounds, reproducibility, MS/MS spectral quality, and detection sensitivity for low-abundance active constituents. Results demonstrated that the DDA mode yielded a higher total number of detected compounds, whereas the DIA mode generated a greater proportion of high-confidence identifications (10.63 % with spectral match scores >0.8). Notably, the DIA approach exhibited significantly superior reproducibility in retention time and peak area for six representative compounds, with rutin showing >3-fold difference in retention time RSD between the two acquisition modes. However, DDA produced cleaner MS/MS spectra with distinct fragment ions, whereas DIA spectra exhibited interference from contaminant ions. Concurrently, DIA effectively detected low-abundance active constituents whose ion chromatograms and MS/MS fragments could not be extracted in DDA mode. This study contributes critical experimental evidence and analytical datasets to inform the selection of high-resolution mass spectrometry acquisition modes for complex TCM formulation research. Subsequent researchers may integrate the complementary advantages of both approaches to achieve dual objectives in comprehensive compound characterization.
    DOI:  https://doi.org/10.3791/69227
  23. Anal Methods. 2025 Oct 21.
      Desorption Electrospray Ionization (DESI) is a unique ambient ionization technique in mass spectrometry that operates under atmospheric pressure without the need for vacuum systems, chemical matrices, or extensive sample preparation. These characteristics distinguish DESI from conventional ionization methods and enable quasi on-demand molecular analysis directly from native surfaces and tissues, an analytical capability otherwise impractical for many time-sensitive or spatially constrained applications. Since its development by Cooks et al. in 2004, DESI-MS has become an indispensable method for both qualitative and quantitative applications. It operates by propelling charged microdroplets (typically <10 μm in diameter) onto sample surfaces, producing gas-phase ions through soft ionization. This review presents a critical evaluation of DESI performance across a range of uses, including surface profiling, molecular imaging, and in situ diagnostics. DESI-MS allows analysis rates exceeding 2 samples per second in formats such as 96-well plates, with detection limits in the low nanogram range. Imaging applications have demonstrated spatial resolutions below 200 μm, with scan speeds reaching 100 μm s-1, enabling detailed molecular mapping in biological tissues. Technological advancements, such as infrared laser-assisted DESI (IR-LADESI), enclosed DESI modules, and microdroplet-driven reaction screening, have expanded DESI's applicability across pharmaceutical, clinical, forensic, and environmental fields. This review synthesizes developments from 2020 to 2025, emphasizing technical principles, instrumentation progress, and analytical performance, and positions DESI-MS as a leading tool in modern mass spectrometry.
    DOI:  https://doi.org/10.1039/d5ay01323b
  24. Mikrochim Acta. 2025 Oct 24. 192(11): 754
      The design and synthesis of Fe3O4@PDA@poly(AA-co-EGDMA) nanoparticles (NPs) as a novel magnetic solid-phase extraction (MSPE) material for efficient enrichment and detection of synthetic cannabinoids (SCs) of various structures in large-volume wastewater is reported. The Fe3O4@PDA@poly(AA-co-EGDMA) NPs were synthesized via a two-step process involving dopamine polymerization and functionalization with poly(acrylic acid-co-ethylene glycol dimethacrylate) polymers, providing hydrophobic and acidic functional groups for enhanced analyte adsorption. An MSPE-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and optimized for the detection of 24 SCs in wastewater. The method exhibited excellent analytical performance with good linearity (R > 0.99), low limits of quantification (LOQ, 0.02-0.1 ng/L), and good precision with recoveries ranging from 50.20 to 92.72%. The method is capable of reliably analyzing trace SCs in large volume samples (300 mL and 1 L). This study introduces a simple, rapid, and cost-effective MSPE-UPLC-MS/MS approach for detecting SCs in complex environmental samples. The proposed method offers significant potential for wastewater-based epidemiology (WBE) applications, providing a valuable tool for monitoring drug use trends, public health surveillance, and regulatory enforcement.
    Keywords:  Magnetic nanosorbent; Magnetic solid phase extraction (MSPE); Synthetic cannabinoids (SCs); Ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS); Wastewater analysis
    DOI:  https://doi.org/10.1007/s00604-025-07578-z
  25. J Vis Exp. 2025 Oct 03.
      Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-ToF MS) is an effective analytical tool for characterizing synthetic polymers, offering precise molecular weight determination and structural insights such as repeat unit masses and end-group identification. This protocol details the steps for polymer analysis, including sample preparation with appropriate matrix and cation selection, data acquisition, and a calibration method to ensure accurate mass measurements. It highlights the versatility of MALDI-ToF MS in analyzing polymers, from monodisperse to highly disperse materials, while observing limitations in resolving highly disperse samples. By comparing theoretical and observed masses, including isotopic patterns, the method enables confident confirmation of repeat units and end groups. The protocol supports new users by presenting representative data on matrix selection, spectral interpretation across dispersity ranges, and characterization of polymers with unique isotopic features or metastable ion formations. Troubleshooting strategies include addressing issues such as matrix interference and samples that ionize without an added cation during sample preparation. Overall, this guide serves as a foundation for using MALDI-ToF MS as a rapid and reliable technique for polymer analysis.
    DOI:  https://doi.org/10.3791/68455
  26. Anal Chim Acta. 2025 Dec 08. pii: S0003-2670(25)01086-4. [Epub ahead of print]1378 344692
       BACKGROUND: Multivariate calibration models in analytical chemistry often suffer from matrix effects due to variations in sample composition and instrumental conditions. These effects present a major challenge, often resulting in inaccurate predictions due to spectral differences and concentration mismatches between unknown samples and calibration datasets. Existing strategies, such as standard addition and local modeling, are limited in addressing both aspects simultaneously. There is a critical need for a systematic approach that enhances calibration model robustness by ensuring spectral similarity and concentration alignment, thereby improving prediction accuracy across diverse sample matrices.
    RESULTS: We developed a matrix-matching procedure using Multivariate Curve Resolution-Alternating Least Squares (MCR-ALS) to enhance the accuracy and robustness of multivariate calibration models. Spectral matching is assessed via net analyte signal (NAS) projections and Euclidean distance, isolating analyte and non-analyte contributions. Additionally, concentration matching is performed by evaluating the alignment of predicted concentration ranges between unknown samples and calibration sets, ensuring consistency across varying sample compositions. The method was rigorously validated using both simulated datasets and real-world analytical data, including near-infrared (NIR) spectra of corn and nuclear magnetic resonance (NMR) spectra of alcohol mixtures. In all tested scenarios, the matrix-matching procedure successfully identified optimal calibration subsets that minimized matrix effects. This approach led to substantially improved prediction performance by effectively reducing errors caused by spectral shifts, intensity fluctuations, and concentration mismatches, outperforming conventional calibration strategies in diverse and complex matrices.
    SIGNIFICANCE: This MCR-ALS-based matrix-matching framework enhances multivariate calibration by systematically selecting calibration sets that match spectrally and in concentration with unknown samples. By minimizing matrix-induced errors, it ensures robust and accurate predictions. Its versatility across analytical platforms and ability to handle diverse matrix effects make it a valuable tool for analytical chemistry, with potential for broad application in real-world analytical challenges.
    DOI:  https://doi.org/10.1016/j.aca.2025.344692
  27. Biomed Chromatogr. 2025 Dec;39(12): e70235
      This study aimed to develop a high-throughput and high-sensitivity method for simultaneously determining trimethoprim (TMP), sulfamethoxazole (SMX), and its metabolite acetyl-N-sulfamethoxazole (NSMX) in critically ill patients' plasma. The samples were precipitated using methanol and then purified using the Oasis PRiME HLB solid-phase extraction column. The mobile phase consisted of a mixture of 40% 0.1% formic acid aqueous solution and 60% acetonitrile, with a flow rate of 0.35 mL/min. Analyses were conducted using UPLC-Q-Exactive Plus Orbitrap mass spectrometry in positive ion mode. With only 50 μL of plasma required for accurate quantification, this method was applicable for therapeutic drug monitoring (TDM). Validation demonstrated precision and accuracy within 15% of nominal values. The samples remained stable for 12 h at 4°C and -20°C and for 15 days at -20°C and -80°C, which ensured the reliability of the method during sample storage and handling under different environmental conditions. The method can be applied for concentration monitoring and pharmacokinetic studies, enabling TDM and dose adjustments for critically ill patients. This approach will enhance patient outcomes and reduce medical resource waste, offering reliable sensitivity and specificity to support precision medicine in critical care.
    Keywords:  UPLC‐Q‐Exactive Plus Orbitrap mass spectrometry; acetyl‐N‐sulfamethoxazole; critically ill patients; sulfamethoxazole; therapeutic drug monitoring; trimethoprim
    DOI:  https://doi.org/10.1002/bmc.70235
  28. Sci Data. 2025 Oct 20. 12(1): 1654
      This Data Descriptor reports the submission of a High-Resolution Orbitrap Mass Spectral Library of Pyrrolizidine Alkaloids (PASL) to public repositories. The library contains 165 tandem mass spectra (MS/MS) from 84 pyrrolizidine alkaloid (PA) standards, along with 18 additional PAs manually annotated in crude plant extracts. This collection comprises most commercially available PAs and a unique selection of annotated (in crude extracts) and synthesized compounds. The PASL serves as a valuable resource for identifying PAs in complex mixtures without analytical standards and facilitates the annotation of novel PAs through molecular networking approach. To ensure high quality, the library was validated by dereplicating its spectra against the GNPS libraries and applying it to the annotation of two PA-producing plant species. The spectra of the PASL can be accessed through GNPS ( https://gnps.ucsd.edu/ProteoSAFe/gnpslibrary.jsp?library=PYRROLIZIDINE-ALKALOID-SPECTRAL-LIBRARY ), with accession numbers ranging from CCMSLIB00014205782 to CCMSLIB00014205946 . The PASL in .mgf format can be downloaded from GNPS under: https://external.gnps2.org/gnpslibrary . The PASL enables rapid and straightforward annotation of both known and novel PAs, accelerating research in food safety and related fields.
    DOI:  https://doi.org/10.1038/s41597-025-05940-7
  29. MethodsX. 2025 Dec;15 103666
      This study presents a comparison of three mass spectrometry-based analytical approaches-targeted tandem mass spectrometry (MS/MS), high-resolution full scan (HRFS), and data-independent acquisition (DIA)-for the quantification and screening of 74 pharmaceuticals across four environmental water matrices: tap water, river water, and influent and effluent wastewater. The methods were validated in terms of limits of quantification (LOQ), trueness, precision, and matrix effects. MS/MS exhibited the best overall performance, achieving the lowest LOQs (median 0.54 ng/L), highest trueness (median 101 %), and minimal matrix effects, confirming its suitability for routine regulatory monitoring. HRFS and DIA, while showing higher LOQs and variability, provided broader screening capabilities with acceptable trueness for 63 % and 81 % of compounds, respectively, and enabled retrospective data analysis. The methods were applied to real samples from the Živný Stream in the Czech Republic to determine pharmaceutical contamination downstream of a wastewater treatment plant (WWTP).
    Keywords:  Mass spectrometry; Matrix effects; Pharmaceuticals; Wastewater; Water analysis
    DOI:  https://doi.org/10.1016/j.mex.2025.103666
  30. Front Cell Infect Microbiol. 2025 ;15 1584487
      Short-chain fatty acids (SCFAs), which are produced by microorganisms in the digestive tract of animals, play an important role in maintaining homeostasis in the host, including immune function. Different types of SCFAs are produced by different intestinal bacterial communities. However, visualizing their spatial distribution within tissue sections has been difficult. This is primarily due to the volatility of SCFAs, which makes detection challenging, even with matrix-assisted laser desorption/ionization (MALDI) mass spectrometry imaging (MSI) using an atmospheric pressure ion source. To address this issue, we minimized the volatility of SCFAs in fresh tissue sections. Then, we used N,N,N-trimethyl-2-(piperazin-1-yl)ethan-1-amine iodide (TMPA) and 1-((dimethylamino)(dimethylimino)methyl)-1H- [1,2,3]triazolo[4,5-b]pyridine-3-oxide hexafluorophosphate (HATU) to chemically derivatize the carboxylic acid into a quaternary amine. This in situ derivatization enabled visualization of SCFAs using MALDI-MSI. In the cecum of mice, strong signals for butyrate and propionate were detected in areas with high bacterial density, as identified by hematoxylin staining. This indicates that these SCFAs are produced by bacteria. Anaerobic bacteria were cultured from the cecum of another individual raised under the same environment. Strain identification was performed using MALDI mass spectrometry of bacterial protein finger prints which confirmed the presence of bacteria that produce SCFAs. This approach, which combines minimizing volatility and in situ derivatization, provides a powerful tool for elucidating the spatial relationship between intestinal bacteria and metabolites including SCFAs.
    Keywords:  HATU; MALDI; MSI; SCFAs; TMPA; proteotyping; short-chain fatty acids
    DOI:  https://doi.org/10.3389/fcimb.2025.1584487