bims-mascan Biomed News
on Mass spectrometry in cancer research
Issue of 2026–06–21
25 papers selected by
Giovanny Rodríguez Blanco, Uniklinikum Graz



  1. Anal Chem. 2026 Jun 15.
      A self-driving metabolomics laboratory has long been envisioned but remains largely unrealized due to the complexity of analytical method design. As an initial step toward this goal, we developed BAGO, a self-optimizing framework for automated liquid chromatography (LC) gradient design in mass spectrometry-based untargeted metabolomics. BAGO aims to enhance global metabolite detection by improving the separation of all compounds, regardless of whether their identities are known or unknown. It operates through a data-driven Bayesian optimization process that iteratively learns from acquired MS data to propose improved gradients. To support this, we propose a global separation index that quantifies coelution among both annotated and unannotated features, enabling robust and structure-agnostic optimization across diverse sample types. Benchmarking across four metabolomics assays involving diverse sample matrices, column chemistries, and gradient durations, BAGO achieved substantial improvements within only 10 optimization iterations by balancing exploration and exploitation. The optimized gradients led to increased numbers of Gaussian-shaped peaks, higher MS/MS acquisition rates, and more annotated metabolites using both identity and analog search approaches. We further applied BAGO to a sex-differentiated metabolomics study of Drosophila abdominal carcasses, completing the workflow in parallel under both initial and optimized gradients. The optimized method resulted in a 41.9% increase in Gaussian-shaped peaks, a 36.8% increase in MS/MS-acquired peaks, and the identification of 18 additional biologically significant metabolites, including sex-associated compounds such as octopamine and pyroglutamic acid. BAGO (https://github.com/HuanLab/bago) is freely available as an open-source tool and represents a generalizable step toward fully automated, self-optimizing experimental workflows in untargeted metabolomics.
    DOI:  https://doi.org/10.1021/acs.analchem.6c01208
  2. STAR Protoc. 2026 Jun 18. pii: S2666-1667(26)00297-2. [Epub ahead of print]7(3): 104644
      Urinary sphingolipids may serve as biomarkers of renal diseases. Here, we present a high-throughput, automated protocol for solid-phase extraction and tandem mass spectrometry (LC-MS/MS) quantification of lipids from urine. We describe steps for sample preparation and lipid extraction, and then detail procedures for targeted LC-MS/MS analysis of urinary sphingolipids. In this protocol, we focus on the analysis of urine samples; however, this platform can be optimized for alternative biospecimens. Additionally, this method allows for tandem preparation of metabolomic and lipidomic samples. For complete details on the use and execution of this protocol, please refer to Nicholson et al.1.
    Keywords:  Health Sciences; High Throughput Screening; Metabolism; Metabolomics; Protocols in Metabolomics and Lipidomics
    DOI:  https://doi.org/10.1016/j.xpro.2026.104644
  3. Lab Chip. 2026 Jun 15.
      Proteomic sample preparation for liquid chromatography-tandem mass spectrometry (LC-MS/MS) is increasingly addressed by automated approaches. However, in clinical settings for precision medicine, where a limited number of samples must be processed in a standardized and reproducible manner with minimal user interaction, fully automized workflows remain scarce. Here, we present the AutoPAC-disk, a centrifugal microfluidic implementation of a protein aggregation capture (PAC) sample preparation workflow for bottom-up proteomics that automates all necessary steps for on-bead proteolysis including on-disk pre-storage of buffers. Comparative evaluation of the AutoPAC-disk using HEK293 cell lysates against a manual reference workflow and a semi-automated robotic PAC implementation showed 50% and 37% more peptide identifications and 23% and 10% more protein group identifications, respectively, while maintaining high quantitative reproducibility as reflected by protein-group intensity coeffincients of variation (CVs) below 10%. Additional analysis demonstrated that the AutoPAC-disk primarily increased identifications of low-abundance proteins without introducing method specific physicochemical bias. The AutoPAC-disk was subsequently evaluated using patient-derived formalin-fixed paraffin-embedded (FFPE) prostate tumor tissue. The AutoPAC-disk yielded 8% more peptide identifications and 10% more protein groups than the manual workflow, with protein-group intensity CVs below 7% for both methods. Together, these results demonstrate that centrifugal microfluidic automation with on-disk buffer pre-storage can substantially simplify proteomic sample preparation, minimize user interaction and lower operational barriers for personnel with limited experience in proteomic sample preparation, providing a promising strategy for clinical and translational proteomics in the field of precision medicine.
    DOI:  https://doi.org/10.1039/d6lc00211k
  4. J Pharm Biomed Anal. 2026 Jun 13. pii: S0731-7085(26)00280-3. [Epub ahead of print]280 117612
      Metabolites of the tricarboxylic acid (TCA) cycle play crucial roles in cancer biology, and their accurate quantification is essential for understanding energy metabolism, signaling dynamics, and identifying metabolic vulnerabilities in cancer cells. However, traditional liquid chromatograph-tandem mass spectrometry (LC-MS/MS) methods for these polar metabolites often encounter challenges, such as limited retention on reversed-phase columns and ion suppression. This study developed and validated two LC-MS/MS methods for the accurate quantification of seven key TCA cycle metabolites in MDA-MB-231, M67-2 (MEMO1 knockdown), and M67-9 (MEMO1 knockout) breast cancer cell lines. For five metabolites, namely citrate (CA), L-malate (MA), fumarate (FA), α-ketoglutarate (AKG), and glutamate (GA), an isotope-coded derivatization approach utilizing 12C/13C-labeled dimethylaminophenacyl (DmPA) bromide was employed to develop a targeted high-performance liquid chromatography (HPLC)-MS/MS method. Inefficient DmPA derivatization in aqueous matrices was addressed by optimizing sample preparation in non-aqueous conditions, and the presence of multiple peaks of AKG was resolved by selecting triethanolamine (TEOA) as the reaction base to improve specificity. Conversely, due to persistent interferences with DmPA derivatization, pyruvic acid (PA) and succinic acid (SA) were quantified using another novel hydrophilic interaction liquid chromatography (HILIC)-MS/MS method in their native underivatized forms. Both methods were validated according to regulatory bodies, ensuring linearity, accuracy, precision, selectivity, and stability. The methods ensured the utilization of two multiple reaction monitoring (MRM) transitions to enhance specificity. The validation approach was adjusted to fit tissue culture studies. The validated methods were successfully used to measure the TCA metabolites in tested cell lines, providing valuable tools for investigating metabolic dynamics in cancer research.
    Keywords:  Cancer cells; DmPA derivatization; HILIC-MS/MS; HPLC-MS/MS; LC-MS/MS; TCA cycle metabolites; Targeted metabolomics
    DOI:  https://doi.org/10.1016/j.jpba.2026.117612
  5. Anal Chem. 2026 Jun 16.
      Methods for unknown metabolite characterization rely heavily on one or more of the following: spectroscopic approaches; tandem mass spectrometry (MS/MS); ion mobility or liquid chromatography; and/or guided intervention through reverse metabolomics, derivatization, etc. The limitations of these methodologies vary widely. For example, spectroscopic approaches are slow and limited in throughput as they necessitate metabolite purification. Additionally, tandem mass spectrometry is often insufficient for unambiguous identification, and guided interventions can be limited in scope. A complementary approach to high-resolution mass spectrometry that is high-throughput, is robust, and provides nondiscrete data (i.e., unique reaction rate) that can rationally inform metabolite structure is desirable. Here, we present an optimized method utilizing sodium bicarbonate for hydrogen-deuterium exchange (HDX) to label slowly exchanging and labile sites over time, after which back-exchange of all labile sites leaves only slowly exchanging sites labeled for subsequent MS analysis. The exchange kinetics and extent of deuterium incorporation aid in metabolite structure identification. The myriads of different metabolite structures impart differences in resonance, inductive, and stearic effects at the labeling site and are resolvable kinetically. This methodology is used to identify different functional groups and provide kinetic resolution of structural isomers (methyl xanthine and methyl 2-oxovalerate as well as ortho, para, and meta isomers of hydroxyhippurate), complemented with density functional theory (DFT) calculations.
    DOI:  https://doi.org/10.1021/acs.analchem.6c00110
  6. Nature. 2026 Jun 17.
      A detailed, spatially resolved quantitative map of the human proteome is essential for a deeper understanding of human biology and disease1-4. Here we present a comprehensive human proteomic landscape, generated by profiling more than 13,000 proteins across 2,856 samples using data-independent acquisition mass spectrometry. The dataset spans 58 major tissue types, 251 specific tissue subtypes and 25 distinct carcinomas. This resource enables the depiction of spatially resolved proteome trajectories across tissue types and physiological states, including fetal, tumour, adjacent non-tumour and healthy adult tissue, thereby providing insight into both developmental processes and oncogenic progression. Furthermore, quantitative proteomics comparisons across diverse tissue types and states facilitate the indication of organ-specific toxicity, the identification of repurposable anticancer drug candidates and the prioritization of therapeutic targets for cancers. This study establishes a quantitative resource for navigating the proteome in the human body and in common cancers.
    DOI:  https://doi.org/10.1038/s41586-026-10660-y
  7. J Proteome Res. 2026 Jun 18.
      Filter-Aided Sample Preparation (FASP) is a well-established method in proteomics, yet its potential for the parallel recovery of metabolites remains largely unexplored. Herein, we evaluate the performance of FASP as a straightforward workflow for the simultaneous isolation of protein and corresponding metabolite fractions from a single urine sample. The FASP-based LC-MS/MS approach for both proteomics and metabolomics analysis identified 3,163 nonredundant peptides corresponding to 957 unique protein groups. The metabolomic profile comparison of three urine fractions, specifically FASP-concentrated, FASP flow-through, and raw samples, resulted in the identification of 176 common metabolites. Next, as a proof-of-concept, the FASP protocol was applied to compare the metabolomic profiles of clinical urine samples from healthy individuals (n = 13) and patients with Ta bladder cancer (n = 12). The metabolomic modulation was consistent with previously reported findings, highlighting perturbations in phenylacetate, purine, and tryptophan metabolism, as reflected by changes in metabolites such as adenosine monophosphate (AMP), phenylacetic acid, glutamine, cytosine, and l-tryptophan. FASP protocol can be effectively adapted for the concurrent profiling of both proteomic and metabolomic fractions from urine samples. Thus, FASP-based workflow represents a viable alternative for single-step sample preparation, facilitating subsequent quantitative multiomics data integration.
    Keywords:  Bladder cancer; FASP; Metabolomics; Multiomics; Proteomics; Sample preparation; Urine
    DOI:  https://doi.org/10.1021/acs.jproteome.6c00173
  8. Protein Sci. 2026 Jul;35(7): e70673
      Maintaining mitochondrial integrity and function is fundamental to cellular homeostasis. Cells rely on coordinated protein quality control (QC) systems-including intricate chaperone-protease networks, the ubiquitin-proteasome system, and cytosolic surveillance pathways-that together form a dynamic, cell-wide mitostasis network governing the import, folding, synthesis, and degradation of mitochondrial proteins. Disruption of mitochondrial homeostasis, for example, by impairing mitochondrial protein import, induces proteotoxic stress and contributes to human disease. Mass spectrometry (MS)-based proteomics has established itself as an indispensable method to dissect mitostasis at unprecedented depth by enabling systematic quantitative analysis of protein abundance, localization, interactions, stability, and dynamics. In this review, we highlight state-of-the-art MS technologies and multifaceted proteomics approaches used to study mitostasis on a proteome-wide level. These functional analysis approaches build on quantitative MS methods employing label-free, metabolic, and chemical labeling strategies, which allow precise tracking of proteome dynamics in response to different cellular conditions including stress. Spatial and interaction-based approaches, such as affinity purification-MS, proximity labeling, and complexome profiling, provide detailed insight into the organization and regulation of the complex mitochondrial organizing system, chaperone networks, and protein QC pathways. Furthermore, we discuss advanced methodologies such as nascent chain and dynamic proteomics strategies, which offer a proteome-wide comprehension of early stress responses and fast regulation. The skillful integration of temporal, spatial subcellular, interaction, nascent, and dynamic proteomics approaches now enables a systems-level assessment of mitostasis, paving the way for a holistic while nuanced understanding of this essential cellular process and the underlying molecular mechanisms.
    Keywords:  complexome profiling; dynamic SILAC; interactome analysis; mitochondria; nascent proteomics; protein import stress; proteome dynamics; proteostasis; proximity labeling; quantitative mass spectrometry
    DOI:  https://doi.org/10.1002/pro.70673
  9. Cell Rep. 2026 Jun 17. pii: S2211-1247(26)00577-2. [Epub ahead of print]45(6): 117499
    Alzheimer Gut Microbiome Project Consortium
      The etiology of Alzheimer's disease (AD) remains unclear but is likely driven by gene-environment interactions. We present a multi-organ untargeted metabolomics atlas (n = 2,271) paired with metagenomics data (n = 666) from two AD transgenic mouse models (3xTg and 5xFAD) under colonized and germ-free conditions. Systems-level analyses revealed clusters of dysregulated molecules across tissues, including carnitines, bile acids, B vitamins, neurotransmitters, and N-acyl lipids. Metabolic shifts were associated with the depletion of Akkermansia muciniphila and enrichment of Mucispirillum schaedleri in the 3xTg model. We identify previously unexplored carnitines linked to microbial metabolism of phenylalanine. Using tissueMASST-a mass spectrometry search tool we developed to translate animal-model findings into a human clinical context-we trace phenylacetyl-carnitine in human plasma and serum samples (n = 1,470) from independent cohorts, revealing associations with aging, cognitive impairment, and diminished memory performance. This public resource and associated tools will aid future research in AD etiology.
    Keywords:  3xTg; 5xFAD; Alzheimer's disease; CP: metabolism; CP: neuroscience; metagenomics; tissueMASST; untargeted metabolomics
    DOI:  https://doi.org/10.1016/j.celrep.2026.117499
  10. J Exp Clin Cancer Res. 2026 Jun 17.
      Lipid desaturation is a fundamental biochemical process essential for maintaining membrane fluidity, energy storage, and cellular signaling. It is increasingly recognized that this homeostatic network is frequently dysregulated by malignant cells to support proliferation, evade programmed cell death, and facilitate immune evasion. There are two primary lipid desaturation pathways: the conversion of saturated fatty acids (SFAs) to monounsaturated fatty acids (MUFAs) by stearoyl-CoA desaturase 1 (SCD1), and the biosynthesis of long-chain polyunsaturated fatty acids (LC-PUFAs) via the fatty acid desaturases (FADS). This review explores how tumors utilize the SCD1 axis to mitigate lipotoxic endoplasmic reticulum (ER) stress and ferroptosis. Furthermore, we discuss how the FADS axis presents a distinct metabolic paradox: while it promotes oncogenic signaling and structural plasticity, it concurrently creates an actionable vulnerability to ferroptosis by enriching membranes with peroxidation-prone PUFAs. This metabolic rewiring provides a strong biological rationale for precision therapeutics.We trace the clinical development of desaturase inhibitors, highlighting the recent entry of SCD1 inhibitor, MTI-301, in a Phase 1 clinical trial for solid tumors and the potential repurposing of Aramchol, while detailing how FADS2 plasticity (the "sapienic shunt") drives therapeutic resistance. By integrating these insights into desaturation lipidomics, metabolic modulation via diet-drug interactions, synergistic combination regimens, and stimuli-responsive nanomedicine, we highlight the translational potential of targeting lipid desaturation to overcome metabolic plasticity and treatment resistance in aggressive malignancies.
    Keywords:  Cancer metabolism; ER stress; FADS2; Ferroptosis; Lipid desaturation; MTI-301 (SSI-4); Metabolic plasticity; Precision therapeutics; SCD1; Sapienic shunt
    DOI:  https://doi.org/10.1186/s13046-026-03747-x
  11. J Proteome Res. 2026 Jun 18.
      Determining when bloodstains were deposited remains an unsolved challenge in forensic science, limiting investigators' ability to reconstruct events and verify suspect timelines. Here, we develop a metabolomics-based approach combining liquid chromatography-mass spectrometry (LC-MS) with machine learning to estimate bloodstain age independent of donor-specific variation. Through untargeted analysis and degradation studies, we identified 51 time-dependent biomarkers and transformed their intensities into stable ratios that normalize for individual differences and blood volume. Using samples collected under controlled environmental conditions, we achieve high accuracy for forensically relevant timeframes with prediction errors of ∼7 h for fresh bloodstains and near-perfect classification of samples as recent (<60 h) or aged (>60 h). Validation on two independent data sets confirms strong performance under typical indoor conditions, while highlighting sensitivity to extreme environmental fluctuations. By addressing key biological and technical sources of variability that have hindered translation to practice, this study establishes a robust analytical framework for bloodstain age estimation. The approach offers a practical foundation for future operational implementation and has the potential to substantially improve forensic timeline reconstruction.
    Keywords:  biomarker ratios; bloodstain; chemometric modeling; machine learning; metabolomics; time-since-deposition
    DOI:  https://doi.org/10.1021/acs.jproteome.6c00199
  12. J Proteome Res. 2026 Jun 17.
      Lipoprotein lipase (LPL) is a membrane-bound, water-soluble enzyme that hydrolyzes triglycerides (TAG) into diacylglycerides (DAG), monoacylglycerides (MAG), and free fatty acids (FFA), enabling lipid uptake and energy distribution across tissues. We developed and validated a mass spectrometry-based in vitro assay to quantify LPL activity and assess interindividual variation in serum and plasma samples. Assay conditions were optimized for LPL concentration, calcium chloride concentration, and incubation time to maximize enzymatic activity. Samples were incubated with and without exogenous LPL and analyzed using targeted lipidomics to quantify changes in TAG, DAG, and FFA species. The assay demonstrated high reproducibility in quality control plasma over 10 days. We observed consistent reductions in TAG species and corresponding increases in DAG and FFA species, which varied according to fatty acid composition. Notably, LPL showed reduced catalytic efficiency for TAG and DAG species containing long-chain polyunsaturated fatty acids (PUFAs). Application of the assay to serum samples from 31 healthy volunteers confirmed these substrate-specific patterns, demonstrating the assay's potential to probe LPL function in physiological and pathophysiological states.
    Keywords:  Lipoprotein Lipase; catalytic efficiency; diglycerides; free fatty acids; lipidomics; mass spectrometry; polyunsaturated fatty acids; triglyceride metabolism; triglycerides
    DOI:  https://doi.org/10.1021/acs.jproteome.5c00922
  13. Adv Sci (Weinh). 2026 Jun 16. e75862
      Leader and follower cells drive collective cancer cell migration through distinct and interactive roles, but their specific metabolic signatures remain largely unknown. Here, we developed and applied a workflow that integrates time-lapse imaging, single-cell tracking, microsampling and direct infusion high-resolution mass spectrometry to profile the lipidomes of individually sampled leader and follower cells from highly migratory TNBC lines HCC1143 and HCC38. Approximately 120 metabolites were detected per cell at the MS1 level, and 70 compounds were assigned based on matched MS2 fragments, indicative of detected head-group or side-chain fragment ions. Distinct leader-follower differences emerged in each cell line. HCC38 cells showed increased fatty acids (FA) in leader cells. In addition, alterations in several phosphatidylethanolamine (PE) and diacylglycerol (DG) species between leader and follower cell subpopulations were detected. Alternatively, leader and follower cells in HCC1143 exhibited changes in phosphatidylcholine (PC) species, with PC(34:1) confirmed by a fragment ions at m/z 184.0733. Overall, this study revealed the dynamic lipid metabolism in live migratory cancer cells, and highlights the potential of integrated dynamic imaging and single-cell mass spectrometry for studying functional heterogeneity within leader-follower cancer phenotypes.
    Keywords:  TNBC; collective migration; direct infusion; lipid profiling; live single‐cell; nano‐ESI
    DOI:  https://doi.org/10.1002/advs.75862
  14. Nat Commun. 2026 Jun 19.
      Mass spectrometry-based chemical proteomics enables unbiased assessment of ligand potency and selectivity across the proteome. However, current approaches remain limited by the low throughput of single-compound screening and reliance on pre-synthesized libraries. Here we devise a mechanism-driven "library-versus-proteome" platform that couples dynamic combinatorial libraries with activity-based protein profiling, enabling real-time selection and optimization of ligands in complex biological systems. This approach increases screening throughput by 10- to 20-fold, streamlines library generation, and adopts a "screen first, synthesize later" paradigm. Applying this platform, we discover covalent inhibitors of serine hydrolases including PPME1, ABHD11 and PNPLA6, and reveal uncharacterized roles of PNPLA6 in lipid metabolism and cancer cell proliferation. We further extend the strategy to cysteine-targeting ligands by designing tailored warheads, enabling proteome-wide EC50 profiling of over 2600 ligandable cysteines and yielding inhibitors for NIT2, PRDX5, TXNDC17 and VCP. Focusing on VCP, we uncover a previously unrecognized signaling axis in which GPCR activity modulates activation of the ER stress-induced unfolded protein response. Using a gel-based "library-versus-proteome" assay, we screen over 800 analogues within two days and identify a more potent VCP ligand with nanomolar activity and in vivo antitumor efficacy. This work establishes library-versus-proteome screening as a scalable strategy for ligand discovery.
    DOI:  https://doi.org/10.1038/s41467-026-74672-y
  15. Mass Spectrom Rev. 2026 Jun 16.
      Trapped ion mobility spectrometry (TIMS) is a highly versatile alternative to the more conventional drift tube ion mobility spectrometer (DTIMS). In TIMS, ions are analyzed using an electric field that holds ions stationary against moving gas. In the basic TIMS, ions are accumulated and trapped in the electric field and then eluted over time according to their collision cross section (CCS) as the strength of the electric field is scanned down. The resultant small size and low operating voltage of TIMS compared to prior approaches make it ideal for hybridization with mass spectrometry. Since its introduction and coupling with Time-of-Flight Mass Spectrometry (TOFMS) in 2011, TIMS has been widely and successfully applied in various bioanalytical fields, including proteomics, glycomics, metabolomics, lipidomics, and native mass spectrometry. In particular, the first commercial TIMS-MS instrument introduced by Bruker Daltonics Inc. (timsTOF), launched in 2016, quickly shined as one of the main reference instruments in bottom-up proteomics. The increased peak capacity, resulting from the additional dimension of separation-that is, mobility-leads to mass spectra of reduced complexity and a greater depth of peptide identification. In this retrospective, different designs and operational modes of TIMS will be presented with a focus on the advantages, potentials and challenges of this technology within the fields of the omics sciences, spanning from metabolomics to structural biology, including single cell analysis. Additionally, the newest platforms utilizing TIMS technology will be introduced, with a focus on future applications and direction of the technology.
    Keywords:  PASEF; TIMS; ion mobility
    DOI:  https://doi.org/10.1002/mas.70034
  16. MedComm (2020). 2026 Jun;7(6): e70809
      The adaptation of lipid metabolism in cancer cells, driven by changes in the tumor microenvironment, presents major challenges for cancer therapy. Here, we addressed the problem of altered lipid metabolism and its role in cancer progression and therapeutic resistance. We demonstrate that hypoxia upregulates the key desaturase, stearoyl-CoA desaturase-1 (SCD1), and the lipid droplet (LD) protein PLIN2, thus promoting lipid metabolic adaptation, cell proliferation, migration, and tumor growth. We found that SCD1 and PLIN2 are essential and interdependent for LD formation. PLIN2 supports cell survival under hypoxic and metabolic stress, whereas SCD1 sustains cancer cell proliferation upon reoxygenation. In addition, we found that SCD1 expression in cancer cells affects nonhistone protein deacetylation, whereas PLIN2 expression enhances protein acetylation. Among these proteins, nucleophosmin(NPM1), a tumor suppressor and regulator of p53, was destabilized through SCD1-dependent deacetylation. In addition, SCD1 interacts with NPM1, influences its cellular localization, and recruits histone deacetylase-2 (HDAC2) to the complex. Notably, we observed that knockdown of SCD1 in vitro or its pharmacological inhibition in vivo enhances cancer cell sensitivity to HDAC inhibitors. Our findings underscore the role of SCD1 in reshaping the cellular acetylome and suggest that targeting SCD1 could sensitize cancer cells to HDAC inhibitors, highlighting a promising therapeutic strategy.
    Keywords:  HDACs; NPM1; SCD1; cancer drug resistance; lipid droplets; nonhistone protein deacetylation
    DOI:  https://doi.org/10.1002/mco2.70809
  17. Bone. 2026 Jun 16. pii: S8756-3282(26)00206-1. [Epub ahead of print] 117980
      Glycolysis is widely considered as a major metabolic pathway in several bone-residing cell types, including skeletal stem and progenitor cells (SSPCs) that are essential for bone development, maintenance, and regeneration. However, the contribution of glycolysis to the in vivo function of SSPCs remains unknown. To examine how reduced glycolysis affects SSPC biology, we conditionally deleted phosphofructokinase-2/fructose-2,6-bisphosphatase 3 (PFKFB3), a key regulator of glycolytic flux. PFKFB3 deletion decreased glycolytic flux by at least 30%, but also reduced glucose‑carbon incorporation into glycolysis-branching pathways and tricarboxylic acid (TCA) cycle intermediates. Despite this overall attenuation of glucose metabolism, PFKFB3-deficient SSPCs maintained metabolic homeostasis and their functional properties. Bone mass was also preserved in mutant mice, even under anabolic conditions that are associated with increased glycolytic demand. Mechanistically, metabolic profiling revealed that PFKFB3 knockout SSPCs compensated for reduced glucose utilization by increasing the uptake of amino acids and pyruvate, with pyruvate‑carbon contributing to TCA cycle anaplerosis and amino acid synthesis. Together, these findings demonstrate that SSPCs possess substantial metabolic flexibility, allowing them to adapt to reductions in glucose metabolism by rerouting alternative nutrients to biosynthetic and bioenergetic pathways. This metabolic reprogramming likely represents an adaptive mechanism that helps preserve bone formation under metabolic stress.
    Keywords:  Cell metabolism; Glycolysis; Metabolic flexibility; PFKFB3; Pyruvate; Skeletal stem/progenitor cell
    DOI:  https://doi.org/10.1016/j.bone.2026.117980
  18. Anal Chem. 2026 Jun 17.
      Real-time mass spectrometry (RTMS), the process by which mass spectral data are analyzed during acquisition on a mass spectrometer, is an integral part of mass spectrometer development. Particularly within the fields of proteomics and metabolomics, RTMS has evolved to include the creation of third-party software that interfaces with a mass spectrometer to provide novel acquisition methodologies, such as applications that use the IAPI from Thermo Fisher Scientific. Developing and testing RTMS applications with the use of a mass spectrometer is a slow and expensive process that creates a bottleneck in the laboratory. Here, we present Corona, a virtual mass spectrometer for use in RTMS application development independent of a mass spectrometer. RTMS applications developed with IAPI connect to Corona seamlessly and operate exactly the same as if connected to a physical instrument. In this manner, it is possible to rapidly create and test RTMS applications prior to deployment on a mass spectrometer.
    DOI:  https://doi.org/10.1021/acs.analchem.6c01637
  19. Sci Data. 2026 Jun 13.
      Valosin-containing protein (VCP), a conserved AAA ATPase hexamer, participates in multiple biological processes including ERAD, ubiquitin-dependent degradation by extracting misfolded proteins for proteasomal degradation. Although its interactions with cofactors are well-characterized, and its dysregulation is implicated in multisystem proteinopathy, amyotrophic lateral sclerosis, and cancer, the tissue-specific VCP interactomes underlying its functional versatility remain elusive. Here, we generated HA-N-tagged VCP knock-in mice via CRISPR/Cas9 strategy and performed affinity purification coupled with data-independent acquisition (DIA) mass spectrometry to systematically profile VCP interactors across eight mouse tissues, yielding a high-confidence dataset. We identified 923 robust VCP-binding partners, including established interactors (UBX2B, UFD1, proteasomal subunits) and novel candidates implicated in energy metabolism (TCA cycle, oxidative phosphorylation) and protein quality control (proteasome, ERAD). Notably, we validated the interaction of VCP to two hepatic candidate proteins, DAXX and PRKAG2 (AMPK γ2 regulatory subunit), using HepG2 cells. This study establishes the first in vivo atlas of the VCP interaction network, providing mechanistic insights into its tissue-specific roles and highlighting potential therapeutic avenues for VCP-related disorders.
    DOI:  https://doi.org/10.1038/s41597-026-07626-0
  20. J Am Soc Mass Spectrom. 2026 Jun 15.
      Reference MS/MS libraries remain incomplete due to the vast chemical diversity of metabolites, leaving many spectra from untargeted metabolomics experiments unannotated─the "dark matter" of metabolomics. Machine learning can extend metabolite annotation beyond direct library matches, but its success depends critically on how MS/MS spectra are converted into numerical representations that capture chemically meaningful features while reducing sparsity. Although numerous spectral representations exist, they have not been systematically compared. Using over 71,000 unique compounds with merged-energy MS/MS spectra, we benchmarked a broad set of spectral featurization methods, including fixed and adaptive binning, global-quantile variable-width bins, frequent-peaks representations, spectrum hashing, and learned embeddings such as Spec2Vec, MS2DeepScore, DreaMS, and SpecEmbedding. We further evaluated how vector dimensionality affects performance. A total of 105 neural network models were trained under 5-fold cross-validation to predict Mol2Vec molecular embeddings and retrieve correct structures from a 0.6-million-compound database. Retrieval was assessed at 0.1, 3, and 10 ppm mass tolerances, and a null ranking model was generated to determine expected Top-N accuracy under random candidate ordering. Adaptive binning, frequent-peaks, and DreaMS produced the most accurate embedding predictions. On the test data set, Top-1 retrieval reached 46%, 44%, and 38% for 0.1, 3, and 10 ppm, respectively, with Top-5 accuracies up to 77%. In the CASMI2022 data set, Top-1 performance remained similar at 0.1 ppm but dropped markedly at wider tolerances, reaching only 26% at 3 ppm and 23% at 10 ppm. To ensure reproducibility and broad community applicability, results were further validated on two fully open benchmark data sets, MassSpecGym and Spectraverse, with findings consistent across all three resources. These results underscore clear performance differences among featurization strategies, the strong dependence of retrieval accuracy on mass precision, and the need for evaluation metrics aligned with structure-level annotation tasks.
    Keywords:  machine learning; metabolite annotation; spectral featurization; structure retrieval; tandem mass spectrometry; untargeted metabolomics
    DOI:  https://doi.org/10.1021/jasms.5c00428
  21. Anal Chem. 2026 Jun 16.
      Glutathione conjugation is a key metabolic detoxification pathway, and its downstream products, mercapturic acid conjugates (MACs), may serve as urinary biomarkers of toxicant exposure. However, MAC profiling is hindered by incomplete filtering coverage and the lack of comprehensive spectral and structural databases. To address these limitations, we developed an analytical workflow integrating novel enzymatic deacetylation with ultrahigh-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS)-based neutral loss filtering. The aminoacylase-1-mediated deacetylation provides an orthogonal approach to detect MACs that lack the characteristic neutral loss of 129.0426 Da. Additionally, an in-house MAC library of 734,170 putative structures, combined with an in silico structure annotation tool, facilitated efficient MAC identification. The strategy was validated using 11 MAC standards spiked into urine and applied to urine samples from 15 participants before and after consuming deep-fried foods. A total of 847 features were mapped to at least one MAC structure, exceeding the ∼100 reported in previous studies, with 581 absent from the Human Metabolome Database (HMDB) or PubChem. Postconsumption, 59 MACs increased and 11 decreased, reflecting exposure-related shifts in reactive aldehydes, lipid oxidation products, acylcarnitines, and acyl-CoA intermediates. These findings demonstrate the utility of the workflow for capturing urinary MAC changes associated with deep-fried food consumption and for prioritizing candidate exposure indicators of reactive chemical species for future validation studies.
    DOI:  https://doi.org/10.1021/acs.analchem.5c08181
  22. Anal Chem. 2026 Jun 19.
      Tumor-associated macrophages, pivotal regulators of antitumor immunity, exert dual functions through their tumoricidal M1 and tumor-promoting M2 phenotypes, which are closely linked to their metabolic states. While conventional mass spectrometry imaging (MSI) can characterize the metabolic features of macrophages, it fails to capture dynamic metabolic activity and real-time substrate utilization within individual cells. In this research, we present an integrated approach that couples cell-resolved matrix-assisted laser desorption/ionization (MALDI)-MSI with stable isotope tracing to visualize dynamic metabolic heterogeneity across individual macrophage phenotypes in situ. Using isotopically labeled fatty acids as metabolic tracers, we revealed that M1 macrophages exhibit significantly enhanced synthesis of phospholipids, including phosphatidylethanolamine (PE), phosphatidylinositol (PI), phosphatidylserine (PS), and phosphatidic acid (PA), compared to M2 macrophages, highlighting a polarization-specific metabolic signature linked to their antitumor function. Moreover, we observed that coculture with tumor cells markedly downregulated the levels of newly labeled phospholipids in M1 macrophages. Critically, the pharmacological inhibition of cPLA2, a key enzyme in the phospholipid metabolic pathway, significantly impaired the antitumor efficacy of M1 macrophages. These findings collectively demonstrate the functional importance of phospholipid metabolism in sustaining macrophage-mediated antitumor immunity. We envision that this spatially resolved metabolic tracing strategy will open new avenues for investigating cell-resolved metabolic crosstalk in complex biological environments.
    DOI:  https://doi.org/10.1021/acs.analchem.6c02192
  23. Anal Chem. 2026 Jun 19.
      Histone post-translational modifications (PTMs) alter chromatin dynamics and contribute to the regulation of gene expression in health and disease, yet mass spectrometry-based histone PTM analysis remains constrained by inefficient sample preparation workflows. Here, we develop RIPUP (Rapid Identification of histone PTMs in Underivatized Peptides), a streamlined multiprotease workflow that reduces sample preparation to hours while improving PTM coverage and quantitative accuracy. Systematic evaluation of Arg-C Ultra and a recombinant (r)-Chymotrypsin protease under varied conditions, including standard derivatization with propionic anhydride and tandem mass tag (TMT) labeling, demonstrated that Arg-C Ultra with TMT labeling achieves a detection of total PTM that exceeds Trypsin-based approaches. Using the HiP-Frag computational framework for unrestrictive PTM identification, we discovered that TMT's tertiary amine provides charge compensation that rescues the ionization of negatively charged acylations revealing 58 succinylation and 31 glutarylation sites─a "dark epigenome" largely undetected by propionylation-based methods. Complementary digestion with Arg-C Ultra and r-Chymotrypsin provides orthogonal sequence coverage, enabling the detection of PTMs in H2A variants, linker histones, and regions poorly represented by arginine-specific cleavage alone. In HEK293T cells treated with the pan-sirtuin inhibitor nicotinamide, RIPUP quantified 112 statistically significant peptidoforms (adj p < 0.05), predominantly increasing with the NAM dose (88 up, 24 down). Application of RIPUP to frozen-thawed rat hippocampal sections within a 3 h workflow identified >200 PTMs including H3 K27/K36/K37 methylation, H4 N-terminal acetylation patterns, and H2A K118/K119 ubiquitination. This rapid, high-efficiency platform enables timely discovery of epigenetic mechanisms and accelerates the path from PTM identification to therapeutic target validation.
    DOI:  https://doi.org/10.1021/acs.analchem.6c01147
  24. Anal Chem. 2026 Jun 17.
      Peptide stapling stabilizes bioactive conformations and expands the chemical space of macrocyclic peptide therapeutics. However, competing stapling pathways often generate structurally heterogeneous products, complicating connectivity assignment and quantitative analysis of macrocyclization selectivity. Here, we develop a mass spectrometry (MS)-based analytical platform that enables structural elucidation of stapled peptides and mechanistic interrogation of their formation pathways. The method employs MS-grade proteases to achieve controlled enzymatic linearization of stapled macrocycles under mild conditions, converting rigid cyclic architectures into linear surrogates that are amenable to tandem MS sequencing while preserving staple-dependent connectivity information. When integrated with ion mobility spectrometry, the workflow enables separation and quantitative monitoring of regioisomeric stapled products, allowing direct assessment of site-selective macrocyclization kinetics. Extension of the approach through covalent labeling further demonstrates its ability to localize modification sites within constrained mono- and bicyclic stapled peptides. Together, this platform enables the systematic analysis of stapling connectivity, topology, reaction selectivity, and chemical modification patterns in rigid stapled peptide systems, offering a valuable analytical tool for the characterization and optimization of macrocyclic therapeutics.
    DOI:  https://doi.org/10.1021/acs.analchem.6c01200
  25. Anal Methods. 2026 Jun 11.
      Urinary metabolites and their concentrations serve as biomarkers for identification of metabolic pathways that relate to specific diseases; therefore, fast and accurate quantification of the metabolites in urine is essential in health assessment and diagnosis. As many urinary metabolites are of polar nature, hydrophilic interaction liquid chromatography (HILIC) has been used over the last several years because it offers faster and more reproducible analyses compared to traditional techniques such as reversed-phase chromatography or capillary electrophoresis. In our study, we developed a HILIC method by using a 3 cm analytical column in connection with tandem mass spectrometry detection for quantification of 10 urinary metabolites including creatinine as the reference for normalization. As all tested metabolites contain ionizable functional groups, pH of the mobile phase was optimized to achieve baseline separation of 2 isomeric pairs (1-methyl-4-imidazoleacetic acid/1-methyl-5-imidazoleacetic acid and 1-methylhistidine/3-methylhistidine) and to obtain overall better separation efficiency resulting in a 7 min analysis. The developed method was validated in terms of sensitivity, carry-over, linearity, matrix effects, accuracy, and precision. The metabolite concentrations in healthy subjects determined by the developed method correspond well with the normal reference values found in the literature. Moreover, the method was tested on a small cohort of COVID-19 patients, where it enabled identification of differences in metabolite levels. Thus, the developed method has potential to be used routinely in a diagnostic field for high-throughput analysis of urine samples.
    DOI:  https://doi.org/10.1039/d6ay00400h