bims-metlip Biomed News
on Methods and protocols in metabolomics and lipidomics
Issue of 2026–05–24
29 papers selected by
Sofia Costa, Matterworks



  1. J Vet Diagn Invest. 2026 May 22. 10406387261447261
      Tryptophan metabolites, such as serotonin and kynurenine, are neurotransmitters that play crucial roles in regulating mood, sleep, and various physiologic functions. We developed and validated a robust and sensitive method for the simultaneous quantification of serotonin (5-HT), kynurenine (KYN), and tryptophan (TRP), in feline and canine plasma using electrospray ionization liquid chromatography-tandem mass spectrometry (ESI-LC/MS/MS). Plasma samples underwent protein precipitation followed by chromatographic separation on a reversed-phase C18 column under isocratic elution. The method was validated, assessing linearity, accuracy, precision, recovery, and matrix effects in both cat and dog plasma. The method had high sensitivity, with limits of detection of 0.2 ng/mL for 5-HT, 0.08 ng/mL for KYN, and 2.5 ng/mL for TRP, and limits of quantification of 0.35, 0.22, and 4.2 ng/mL, respectively. Calibration curves showed excellent linearity (R2 > 0.995) across biologically relevant concentration ranges. Intra- and inter-day accuracy and precision were within acceptable limits (<15% relative SD). The method had good recovery and minimal matrix effects. The method was further applied to plasma samples from healthy dogs and cats to demonstrate its applicability to biological samples and to report analyte concentrations in clinically healthy animals. Our validated LC-MS/MS method enables precise and reliable quantification of 5-HT, KYN, and TRP in feline and canine plasma.
    Keywords:  LC-MS/MS; canine plasma; feline plasma; kynurenine; serotonin; tryptophan
    DOI:  https://doi.org/10.1177/10406387261447261
  2. Talanta. 2026 May 09. pii: S0039-9140(26)00612-0. [Epub ahead of print]309 129956
      Sample preparation remains one of the most critical and challenging steps in liquid chromatography - mass spectrometry (LC-MS) metabolomic analysis, as it directly affects metabolite recovery and analytical accuracy and reliability. In this study, we systematically compared solid-phase extraction (SPE) strategies for serum sample preparation in both targeted and untargeted metabolomic approaches. A total of 71 metabolites with diverse structural and polarity characteristics were analyzed using various SPE formats, including dispersive SPE with multiple sorbents and extraction modes, SPE spin columns, SPE pipette tips, and conventional SPE cartridges. Sorbents within the same extraction mode yielded comparable results. Hydrophilic interaction liquid chromatography sorbents demonstrated the highest performance across a wide range of polarities, whereas reversed-phase sorbents favored moderately polar compounds. Ion-exchange sorbents exhibited limited suitability for broad metabolite coverage due to strong pH dependence but improved recovery of ionizable compounds when combined with other sorbents. While different SPE formats showed similar extraction efficiency, their repeatability varied, with spin columns outperforming conventional cartridges. SPE exhibited mitigation of matrix effects in targeted analysis, particularly for highly polar metabolites, compared to protein precipitation (PPT). Although PPT offered higher efficiency in the untargeted workflow, SPE increased feature coverage by up to 50%. Among commercial products, hydrophilic-lipophilic balanced (HLB) sorbents delivered superior efficiency and repeatability, with HLB-packed spin columns providing the most universal and robust performance for LC-MS metabolomic analysis. The results of this systematic evaluation offer practical guidance for selecting appropriate sample preparation strategies tailored to specific analytical goals and target metabolites.
    Keywords:  Mass spectrometry; Metabolomics; Sample preparation; Solid phase extraction; Targeted analysis; Untargeted analysis
    DOI:  https://doi.org/10.1016/j.talanta.2026.129956
  3. Talanta. 2026 May 15. pii: S0039-9140(26)00667-3. [Epub ahead of print]309 130011
      In this work, two computational approaches for metabolite quantification in serum samples using 1H NMR spectroscopy were evaluated: the spectral matching method (MSM) implemented in MagMet and the non-linear least squares method (MNLLS) implemented in Chenomx. The comparison focused on their underlying methodologies, including deconvolution algorithms and user workflows, to assess their relative performance and suitability for metabolomics data analysis. As various analyses (e.g. pattern recognition, classification, biomarker discovery, and pathway analysis) rely on the precision and consistency of input features (e.g., metabolite concentrations), selecting a robust quantification method is essential. Variability in quantification can introduce noise and impact the stability and comparability of analytical outputs. To validate performance, MSM (MagMet) and MNLLS (Chenomx) were benchmarked against quantitative NMR (qNMR) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), the latter serving as the primary reference due to its high sensitivity and broad metabolite coverage (Gika et al., 2014) [1]. Although LC-MS/MS may be affected by matrix effects and ion suppression; these factors are well characterized and routinely mitigated through isotope-labeled internal standards and validated analytical workflows. Moreover, LC-MS offers substantially higher sensitivity than NMR, typically by two to three orders of magnitude, enabling the detection and quantification of hundreds to thousands of metabolites within a single analysis (Nagana Gowda and Raftery, 2022) [2]. qNMR was included as a complementary technique to provide orthogonal validation rather than serving as the sole benchmark. Ten independent serum control samples from a healthy reference group were analyzed to account for natural biological variability, enhancing the generalizability of the findings. The comparison was structured around four criteria: (i) quantitative performance, (ii) computational stability, (iii) usability and processing time, and (iv) method-based similarity via partial least squares-discriminant analysis (PLS-DA). This work differs from prior studies by integrating statistical validation, repeatability testing, and practical usability assessment, and by benchmarking computational quantification pipelines against experimentally grounded methods such as qNMR and LC-MS/MS [3-5]. The selected approach is expected to demonstrate improved consistency in quantification relative to the alternative, contributing to more reliable biological interpretations and more reproducible analytical outcomes across datasets.
    Keywords:  Bioinformatics; Metabolomics; Multivariate analysis; Quantitative NMR
    DOI:  https://doi.org/10.1016/j.talanta.2026.130011
  4. Anal Chem. 2026 May 20.
      Liquid chromatography-mass spectrometry (LC-MS) untargeted analysis enables comprehensive lipid profiling of biological samples. However, system-level interpretation is often limited by the large number of unannotated features. Assigning features to lipid classes provides a higher-level, yet informative, overview that complements detailed structural analysis and supports biological interpretation at the class level. Recent advances in the systematic prediction of chemical class using tandem mass spectrometry (MS2) help address this; however, a substantial proportion of features in untargeted LC-MS data sets are typically characterized only at the MS1 level. Here, we present a workflow to systematically predict the lipid class from MS1-only data in untargeted LC-MS, without requiring prior annotations or MS2. Motivated by previous research showing that Gaussian graphical models (GGMs) estimated from feature intensities can encode the lipid class structure, our method, GgmLipidClassifier (GLC), combines conventional accurate-mass database searching with a GGM-derived network structure in a unified scoring framework to predict lipid class according to the LIPID MAPS Structure Database (LMSD) ontology. Across three human serum and plasma data sets, GLC achieved overall accuracies of 82-90% at the LMSD main class-level and 72-86% at the lipid subclass level, with improved accuracy and reduced uncertainty compared to closest-m/z matching. GLC provides class predictions for most detected features and also generates prediction quality scores to support downstream interpretation. Applied to serum samples from an Alzheimer's disease study, lipid class enrichment based on GLC predictions was highly consistent with class enrichment derived from ground-truth lipid annotations. Importantly, GLC extended coverage to classes missing from the annotation set, revealing biologically plausible associations with Alzheimer's disease, including cholesterol and derivatives, vitamin D3 and derivatives, and plasmalogen glycerophosphoethanolamines. Overall, GLC provides robust lipid class predictions from MS1-only data, generating lipid class assignments for most detected features and complementing conventional analysis to support broader system-level interpretation.
    DOI:  https://doi.org/10.1021/acs.analchem.5c08067
  5. J Chromatogr A. 2026 May 15. pii: S0021-9673(26)00434-6. [Epub ahead of print]1782 467105
      Acylcarnitines (ACs) play a pivotal role in metabolism, most notably by facilitating the transport of fatty acids (FAs) into mitochondria for β-oxidation, a key step in cellular energy production. Dysregulation of AC, FA, and amino acid (AA) levels has been linked to various metabolic disorders, including cardiovascular diseases, neurodegenerative conditions, and cancer. Consequently, monitoring these metabolites in blood samples provides valuable insights into metabolic health and disease progression. In this study, we developed a method for the quantification of carnitine, seven ACs, fifteen FAs, and thirteen AAs in human serum using reversed-phase ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). By employing 3-nitrophenylhydrazine (3-NPH) derivatization, we achieved high detectability for ACs, with limits of detection (LODs) ranging from 0.01-0.27 ng/mL for ACs, 0.22-1.76 ng/mL for FAs and 0.17-18.25 ng/mL for AAs. Recovery rates ranged from 92-126% for ACs, 56-116% for FAs and 86-115% for AAs. Inter- and intra-day precision were below 20% for all metabolites except two FAs. This method provides a reliable and sensitive tool for the simultaneous analysis of ACs, FAs, and AAs in serum, with potential applications in clinical diagnostics and metabolic research.
    Keywords:  Acylcarnitine; Amino acids; Fatty acids; LC-MS/MS; Nitrophenylhydrazine
    DOI:  https://doi.org/10.1016/j.chroma.2026.467105
  6. J Agric Food Chem. 2026 May 21.
      Plant hormones regulate diverse physiological processes, but their simultaneous analysis is challenging due to structural diversity, low abundance, and complex matrices. Herein, we report a chromatography-free analytical platform integrating one-pot dual-channel derivatization with acoustic ejection mass spectrometry (AEMS). Using N,N-diethyl-1,2-ethanediamine for carboxyl-containing hormones and 2-methyl-4-phenylaminomethyl-benzeneboronic acid for cis-diol-containing brassinosteroids, 11 key phytohormones were rapidly derivatized (< 1 min) in a single reaction vessel. The derivatization enhanced sensitivity up to 183-fold, achieving femtogram-level limits of detection (3.9-22 fg). Coupled with AEMS, each sample was analyzed in ∼3 s without chromatography. Validation confirmed excellent linearity (R2 ≥ 0.9991), precision (RSD < 15.3%), accuracy (77.3-110.8% recovery), and minimal matrix effects (76.3-105.1%). The method successfully quantified endogenous plant hormones in Arabidopsis thaliana seeds, Brassica napus stamens, and Oryza sativa seeds, and captured dynamic hormone changes during rice germination. This high-throughput platform provides a promising tool for comprehensive plant hormone profiling.
    Keywords:  acoustic ejection mass spectrometry; chemical derivatization; high-throughput analysis; plant hormones
    DOI:  https://doi.org/10.1021/acs.jafc.6c05085
  7. Int J Vet Sci Med. 2026 ;14 1
       Background: Per- and poly-fluoroalkyl substances (PFAS), known as "forever chemicals," are synthetic compounds widely used for their unique physicochemical properties. Their environmental persistence and potential link to adverse health outcomes have raised significant concerns, necessitating robust monitoring methods. While numerous studies have quantified PFAS in human biological fluids, there is a critical gap in the availability of validated analytical techniques for companion animals remain scares.
    Aims and Objectives: The aim of this study was to develop and validate a novel analytical method for the quantification of eleven PFAS in biological samples from companion animals, specifically canine serum and feline plasma, and to apply this method to real samples.
    Materials and Methods: A streamlined sample preparation protocol was developed including protein precipitation, evaporation under nitrogen at 45°C, and reconstitution. Quantification was performed by ultra-high-performance liquid chromatography-tandem mass spectrometry in negative electrospray mode, monitoring two transitions for each compound.
    Results: The method was validated according to European Medicines Agency guidelines and demonstrated excellent analytical performance, with strong linearity (R² ≥ 0.99), high precision (CV% < 15%), and accuracy within ±15% of nominal concentrations. Recovery ranged from 80.0% to 114.9% and process efficiency from 80.7% to 114.0%, with negligible matrix effects and no observable carry-over. Application to real samples from 23 healthy dogs and 4 healthy cats revealed PFAS concentrations ranging from 0.1 to 15.8 µg/L in dogs and from 0.1 to 2.8 µg/L in cats. PFOS was the most prevalent compound in both species, with PFHxS also prominent in cats.
    Conclusion: The validated UHPLC-MS/MS method provides a reliable and efficient tool for the biomonitoring of PFAS in companion animals. Its application enables large-scale assessment of environmental exposure and supports the evaluation of potential health implications for both pets and their owners.
    Keywords:  Cats; dogs; endocrine disruptor; monitoring; per- and poly-fluoroalkyl substances; sentinels
    DOI:  https://doi.org/10.4103/ijvsm.ijvsm_9_26
  8. Clin Chem Lab Med. 2026 May 19.
       OBJECTIVES: The 20- and 22-kDa isoforms of growth hormone 1 (GH1) play potentially distinct physiological and pathological roles, but their structural similarity makes quantification challenging. Conventional immunoassays lack sufficient specificity, highlighting the need for more precise analytical methods.
    METHODS: We developed a method combining immunocapture with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for precise quantification of GH1 isoforms, with evaluation of sensitivity, accuracy, precision, and linearity. GH1 was isolated from 1-mL serum samples by immunocapture using antibody-coated magnetic beads, eluted, and quantified by LC-MS/MS. Stable isotope-labeled 22-kDa GH1 was used as an internal standard (IS). Clinical applicability was evaluated by analyzing serum GH1 isoforms in 63 patients with somatotroph adenoma.
    RESULTS: The assay demonstrated linear dynamic ranges of 0.2-20.0 μg/L for 20-kDa GH1 and 1.0-100.0 μg/L for 22-kDa GH1. Intra- and inter-assay coefficients of variation were <10 %, and recoveries ranged from 95.0 to 102.5 % after IS correction. Although total GH1 concentrations measured by LC-MS/MS were systematically lower than those obtained by immunoassay, the two methods were strongly correlated (r=0.991, p<0.01). Most patients with somatotroph adenoma (80.0 %; 51/63) exhibited increased 22/20-kDa GH1 ratios, while six patients with unfavorable clinical features and endocrine prognosis exhibited elevated 20-kDa GH1 levels.
    CONCLUSIONS: This immunocapture LC-MS/MS method enables simultaneous quantification of 20- and 22-kDa GH1 isoforms without enzymatic digestion. The implementation of this method may refine the assessment of biochemical remission and prognostic stratification in GH-related disorders.
    Keywords:  human growth hormone; immunocapture; isoform; liquid chromatography-tandem mass spectrometry; somatotroph adenoma
    DOI:  https://doi.org/10.1515/cclm-2026-0382
  9. Anal Methods. 2026 May 22.
      Background: accurate therapeutic drug monitoring (TDM) of β-lactam antibiotics such as meropenem and piperacillin-tazobactam is essential in critically ill patients, where profound pharmacokinetic variability may lead to subtherapeutic exposure or toxicity. Practical, high-throughput analytical workflows are needed to support timely dose optimisation in routine clinical settings. Methods: we developed and fully validated a unified LC-MS/MS method for the simultaneous quantification of meropenem, piperacillin, and tazobactam in human serum. Samples were prepared by protein precipitation and analysed on a C18 column using a water/methanol gradient with 0.1% formic acid. Detection was performed by multiple reaction monitoring with isotopically labelled internal standards. Results: the assay demonstrated excellent linearity (R2 > 0.998), high sensitivity (LLOQ 0.02 mg L-1), and robust intra- and inter-day precision (<10%), with a 10 min run time and no detectable carry-over. The method demonstrates high analytical sensitivity, with a lower limit of quantification (LLOQ) of 0.02 mg L-1 for all analytes, which is among the lowest reported for simultaneous quantification of meropenem, piperacillin, and tazobactam. Application to >40 clinical samples from critically ill patients revealed wide concentration ranges (meropenem 0.2-270 mg L-1; piperacillin 1-580 mg L-1; tazobactam 0.1-60 mg L-1), with unbound fractions consistent with published data. Conclusions: this streamlined, low-volume LC-MS/MS workflow enables rapid, accurate quantification of key β-lactam antibiotics and supports routine TDM in critically ill and paediatric populations, facilitating more individualised antimicrobial dosing in clinical practice. Since our method already accommodates β-lactams and a β-lactamase inhibitor with highly heterogeneous physicochemical properties, it provides a robust basis for extending the approach to additional antibiotics within a multi-analyte framework.
    DOI:  https://doi.org/10.1039/d6ay00331a
  10. Biomed Chromatogr. 2026 Jul;40(7): e70491
      A sensitive and robust ion chromatography method with suppressed conductivity detection (IC-CD) was developed and validated for the simultaneous quantification of six inorganic anions (fluoride, nitrite, bromide, nitrate, phosphate, and sulfate) in animal whole blood. The method employed a carbonate-bicarbonate eluent (4.5-mM Na2CO3, 0.8-mM NaHCO3) at a flow of 1 mL/min and an anion-exchange column (4 × 250 mm, Dionex IonPac AS23 RFIC) to achieve baseline resolution of all analytes within a 30-min run. Sample preparation involved protein precipitation with ice-cold methanol followed by centrifugation, dilution, and filtration. The method demonstrated excellent linearity (R2 = 0.9974-0.9998), with limits of detection (LODs) ranging from 0.27 to 2.96 mg/L. Accuracy was confirmed through recovery studies, yielding values between 99.4% and 118.2%. Intraday and interday precision, expressed as relative standard deviation (%RSD), was consistently below 10% for both peak areas and retention times. The developed IC-CD protocol offers several advantages over existing techniques, including minimal sample volume, simplified sample preparation, rapid analysis, and high reproducibility. This method provides a valuable application tool for assessing ionic balance, nutritional status, and environmental exposure in animal health monitoring and toxicological studies.
    Keywords:  anion profiling; ion chromatography; method development and validation; suppressed conductivity detection; veterinary toxicology; whole blood
    DOI:  https://doi.org/10.1002/bmc.70491
  11. Trends Analyt Chem. 2026 May;pii: 118767. [Epub ahead of print]198
      Achieving high-spatial-resolution in ambient mass spectrometry imaging (MSI) is critical in accurately characterizing the spatial distribution of biomolecules. Ambient MSI enables in situ mapping spatial heterogeneity of metabolites under ambient conditions, facilitating molecular imaging from multicellular structure down to subcellular level. In this review, we first summarized the strategies developed to enhance spatial resolution in ambient MSI, including technological innovations, advances in sample preparation, and data-driven approaches. We then discussed the applications of these techniques in metabolomics studies and addressed current challenges and limitations. Finally, we highlighted emerging opportunities and future directions for achieving ambient high-spatial-resolution MSI.
    Keywords:  ambient MSI; high-spatial-resolution; lipidomics; mass spectrometry imaging (MSI); metabolomics
    DOI:  https://doi.org/10.1016/j.trac.2026.118767
  12. J Pharm Biomed Anal. 2026 May 19. pii: S0731-7085(26)00241-4. [Epub ahead of print]279 117573
      Feature-Based Molecular Networking (FBMN) is a robust strategy for the structural elucidation of natural products; however, inconsistent workflows across software platforms and ionization modes hinder its standardized application. This study systematically evaluated six FBMN construction approaches using LC-MS/MS data acquired from secondary metabolites produced by Lespedeza bicolor-associated endophytic fungi. We compared the MZmine and GNPS (Global Natural Products Social Molecular Networking, https://gnps.ucsd.edu) platforms across positive and negative ionization modes, as well as across different data integration strategies. The results indicated that platform selection and ionization polarity significantly influenced network topology and annotation efficiency. The MZmine-based data-level merged network exhibited superior performance in node density and overall metabolite coverage. Conversely, the GNPS-based network-level merging strategy was more effective in grouping unknown metabolites and facilitating structural interpretation. Positive ionization consistently yielded a higher number of annotations and better annotation accuracy than negative mode, while dual-polarity integration significantly enhanced network connectivity. Specifically, GNPS network-level merging strengthened spectral-similarity linkages, whereas MZmine data-level merging maximized the representation of chemical diversity. These findings demonstrate that a combinatorial approach, integrating dual ionization modes and complementary FBMN platforms, is essential for optimizing metabolite identification in complex natural product matrices.
    Keywords:  Feature-based molecular networking; Ion mode; Merged network; Metabolite annotation; Untargeted metabolomics
    DOI:  https://doi.org/10.1016/j.jpba.2026.117573
  13. Food Chem. 2026 May 15. pii: S0308-8146(26)01814-5. [Epub ahead of print]518 149656
      Glucosinolates (GSLs) are bioactive secondary metabolites in Brassicaceae plants that contribute to both food flavor and plant defense. Their untargeted profiling is challenging because of the large discrepancy between their high chemical diversity and the limited availability of authentic standards. To address this gap, we developed an in silico mass spectral library containing 142 previously reported and 1776 computationally generated GSL species. The corresponding high-resolution MS/MS spectra were predicted based on fragmentation rules learned from standards. Compatible with NIST MS Search and MS-DIAL, the library enables automatic GSL annotation without the need for chemical standards. Application to 13 Brassicaceae species annotated 107 endogenous GSLs, including 36 unreported candidate species, which markedly expanded known GSL diversity. Distinct GSL patterns reveal species-specific chemical signatures and functional responses to pathogen infection. The library provides a robust structural and mass spectral resource for untargeted GSL profiling, enabling systematic exploration of GSL diversity in plants.
    Keywords:  Brassicaceae plant; Glucosinolate; In silico library; Mass spectrometry; Structural database
    DOI:  https://doi.org/10.1016/j.foodchem.2026.149656
  14. J Am Soc Mass Spectrom. 2026 May 18.
      Mass spectrometry imaging is a powerful technique for mapping the spatial distribution of endogenous and exogenous molecules in biological tissues, but it is limited to relative quantitation. To address this limitation, we developed an integrated approach that combines desorption electrospray ionization mass spectrometry imaging with coulometric mass spectrometry to achieve the absolute quantification of drug molecules at the pixel level, without the use of external standards or isotopic labeling. We applied this method to quantify olanzapine, an antipsychotic drug, and its minor hepatic metabolite, 2-hydroxymethylolanzapine, in rat liver tissue. CMS enabled the electrochemical redox quantification of both compounds extracted from tissue regions of interest as defined by mass spectrometry imaging. This established a direct correlation between the imaging signal intensity and the absolute analyte concentration. Our results demonstrate the robustness and sensitivity of this combined approach and support its potential as a generalizable platform for standard-free, quantitative imaging of biological tissues, thereby converting relative ion maps into fully quantitative molecular images.
    DOI:  https://doi.org/10.1021/jasms.5c00445
  15. Ann Pharm Fr. 2026 May 21. pii: S0003-4509(26)00075-1. [Epub ahead of print]
      Irinotecan (CPT-11; IRN) is used as a potent chemotherapeutic agent for CRC. Co-loaded self-nanoemulsifying drug delivery system (SNEDDS) of IRN with cyclosporine A (CSP), a P-gp inhibitor, was designed and developed. A novel liquid chromatography-triple quadrupole mass spectrometry (LC-QqQ MS/MS) method was developed and validated. The analysis was performed on a TSQ Quantis Plus triple quadrupole mass spectrometer, coupled with a Thermo Vanquish UHPLC system, using an Agilent Eclipse Plus C18 column and a gradient elution using 10mM ammonium acetate (0.1% formic acid) and methanol. Retention times were 6.2 min for IRN and 10.17 min for CSP. Linearity was achieved over the ranges of 10-10,000 ng/mL for IRN and 10-5,000 ng/mL for CSP, with R² values of 0.9999 and 0.9998, respectively. Inter- and intra-day precision values were within acceptable limits, and recoveries were consistently 99-100%. The analytical method was applied for bioanalytical estimation using protein precipitation in MDCK cell permeability studies, and HCT-116 colorectal cancer cell internalization. The method demonstrates high sensitivity, reproducibility, and applicability for evaluating co-loaded SNEDDS formulations of IRN and CSP along with quantitation of IRN in MDCK and HCT-116 colorectal cell lines.
    Keywords:  ICH guidelines; LC-MS/MS; LC–MS/MS; analytical validation; bioanalytical method; cancer colorectal; cell lines; colorectal cancer; directives ICH; lignées cellulaires; method optimization; méthode bioanalytique; optimisation de méthode; self-nanoemulsifying drug delivery system; stability study; système d'administration de médicament auto-nanoémulsifiant; validation analytique; étude de stabilité
    DOI:  https://doi.org/10.1016/j.pharma.2026.05.007
  16. Anal Chem. 2026 May 21.
      Untargeted high-resolution mass spectrometry (HRMS) is widely used in metabolomics, exposomics, and chemical monitoring. However, compound annotation, a central element for interpreting untargeted data, is frequently reported without sufficient information to allow independent evaluation. This communication examines current annotation practices in untargeted HRMS studies and remarks the increasing lack of standardized reporting of metadata, structural identifiers, and confidence criteria. Annotations are often reduced to compound names and exact masses, sometimes relegated to Supporting Information or omitted entirely, despite their central role in data interpretation. Although several community initiatives and guidelines have proposed reporting recommendations and identification confidence frameworks, their application and enforcement remain inconsistent. As a result, annotation traceability is often insufficient to support reproducibility, interstudy comparability, or long-term data reuse. These limitations affect downstream applications, including meta-analyses, automated data mining, and regulatory-relevant fields such as food safety and exposure assessment. This article argues that improving annotation traceability is essential for the scientific robustness of untargeted HRMS workflows and emphasizes the role of journals, reviewers, and authors in ensuring that annotation information remains verifiable, reusable, and scientifically accountable.
    DOI:  https://doi.org/10.1021/acs.analchem.6c00439
  17. Anal Biochem. 2026 May 15. pii: S0003-2697(26)00114-4. [Epub ahead of print] 116158
      Xylazine, an alpha 2 adrenergic agonist approved for veterinary use, has become an increasingly common adulterant in the illicit drug supply and is frequently detected with fentanyl and other substances, exacerbating opioid epidemic. Because xylazine is not included in many routine toxicology screens, a practical quantitative urine method is needed for clinical testing and surveillance. We developed and validated a quantitative dilute and shoot method for xylazine in urine using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with water (containing 0.1% formic acid) and methanol (containing 0.1% formic acid) as the aqueous and organic mobile phase, respectively. The assay was linear from 20 to 5000 μg/L, with administratively set limit of quantitation (LOQ) of 20 μg/L and cutoff of 40 μg/L. In 94 authentic urine samples, 11 were above the LOQ (two of which were below the cutoff), with a maximum concentration of 4298 μg/L. The validated method provides robust quantitative measurement of xylazine in urine across clinically relevant concentrations and is well suited for high throughput clinical toxicology and surveillance testing.
    DOI:  https://doi.org/10.1016/j.ab.2026.116158
  18. MAK Collect Occup Health Saf. 2024 ;9(4): Doc097
    MAK Commission
      The working group "Analyses in Biological Materials" of the German Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area (MAK Commission) developed and verified this biomonitoring method for the determination of urinary concentrations of bis(1,3-dichloropropyl) phosphate (BDCPP), which is the major metabolite of tris(1,3-dichloropropyl) phosphate (TDCPP). TDCPP is one of the most commonly used organophosphate flame retardants in cars, residential furniture, and products containing polyurethane foam, and has been detected in dust from private houses, office buildings, and car interiors, suggesting that a majority of the general population is exposed to TDCPP. The aim of this work was to establish a reliable, selective, and sensitive method for the detection of BDCPP in urine. The urine samples are spiked with the internal standard d10-BDCPP and slightly acidified. Cleanup by mixed-mode anion-exchange solid-phase extraction is applied, and BDCPP is detected by liquid chromatography with simultaneous atmospheric pressure chemical ionisation and electrospray ionisation-tandem mass spectrometry. Calibration is carried out in ultra-pure water ∶ MeOH (4 ∶ 1, v/v). Good precision data with standard deviations below 7%, as well as good accuracy data with mean relative recoveries in the range of 93.6-101%, show that the method provides reliable and accurate analytical results. The method is both selective and sensitive, and the limit of quantitation of 0.2 ng BDCPP/l urine is sufficient to determine occupational exposure as well as higher background exposure levels to TDCPP in the general population.
    Keywords:  BDCPP; LC-APCI-ESI-MS/MS; TDCPP; biomonitoring; flame retardant; urine
    DOI:  https://doi.org/10.34865/bi72236e9_4or
  19. Anal Methods. 2026 May 15.
      Conventional multiple reaction monitoring (MRM) quantification of β-agonists in complex matrices was hindered by insufficient sensitivity due to co-extracted matrix interferents. To address this drawback, we developed a highly selective and specific liquid chromatography triple-stage tandem mass spectrometry (LC-MS/MS/MS, LC-MS3) method via systematic comparison of MRM and MRM3 modes for the determination of nine β-agonists (ractopamine, penbutolol, cimaterol, salbutamol, clenbuterol, tulobuterol, clorprenaline, terbutaline, and fenoterol) in high-fat milk and pork. The MS3 method overcomes the limitations of conventional MS/MS through the multi-stage fragmentation capability of a hybrid linear ion trap (LIT), enabling deeper structural characterization and superior matrix interference resistance. The results demonstrated that the LC-MS3 method not only accurately quantified β-agonists in complex matrices, but also significantly enhanced sensitivity by reducing matrix effects. Extracted ion chromatograms (XICs) revealed nearly interference-free peaks, exhibiting the excellent selectivity and specificity of the LC-MS3 method. The LC-MS3 method exhibited good linearity (R2 ≥ 0.9973), and the limits of detection (LOD) and quantification (LOQ) for β-agonists ranged from 0.01 to 0.05 µg kg-1 and 0.03 to 0.15 µg kg-1, respectively. The recoveries were between 85.47% and 105.32%, with intra-day and inter-day relative standard deviations (RSDs) of 1.68-6.42% and 2.42-8.68%, respectively. The matrix effect (ME) was within -10.55% to 9.53%. In comparison, the conventional LC-MS/MS method showed higher LODs (0.1-0.15 µg kg-1) and LOQs (0.3-0.45 µg kg-1) and broader matrix effects (-18.12-19.35%), confirming the superior sensitivity of the LC-MS3 method. This is the first study to employ MRM3 mode for the determination of β-agonists in high-fat milk and pork matrices.
    DOI:  https://doi.org/10.1039/d6ay00363j
  20. Rapid Commun Mass Spectrom. 2026 Aug 30. 40(16): e70113
       RATIONALE: Neonicotinoid insecticides like clothianidin pose significant ecological risks due to their environmental persistence and toxicity to nontarget organisms. Accurate monitoring of ultratrace residues in complex biological matrices is essential for risk assessment. This study aims to develop a highly selective analytical platform to overcome matrix interferences and sensitivity limitations inherent in traditional methods.
    METHODS: A novel method was developed using ultrahigh performance liquid chromatography coupled with triple-stage mass spectrometry (UPLC-MS3) on a QTRAP 6500+ system. Clothianidin was extracted from zebrafish tissues via protein precipitation with acetonitrile. The MS3 transition (m/z 250.1 → 168.9 → 110.0) was optimized to enhance the signal-to-noise ratio compared with conventional multiple reaction monitoring (MRM).
    RESULTS: The UPLC-MS3 method provided a 13-fold improvement in signal-to-noise ratio (713.5) over MRM (54.5). The limit of quantification was 0.05 ng/mL across all tissues. Validation showed excellent linearity (r > 0.995), precision (CV < 8.4%), and recovery (90.64%-111.98%). Exposure studies revealed tissue-specific bioaccumulation, with the highest clothianidin concentrations found in muscle (6.06 ng/mg) and heart (5.42 ng/mg).
    CONCLUSIONS: The developed UPLC-MS3 platform offers unparalleled sensitivity and specificity for trace-level monitoring of clothianidin in complex biological systems. These findings provide a robust tool for investigating the environmental fate and toxicological mechanisms of neonicotinoids in vertebrates.
    Keywords:  UPLC–MS3; bioanalysis; clothianidin; quantification; tissue distribution
    DOI:  https://doi.org/10.1002/rcm.70113
  21. Indian J Psychiatry. 2026 Apr;68(4): 351-357
       Background: Tapentadol, a dual-action opioid, is increasingly misused in India by intravenous injection of crushed tablets. Objective urine testing is scarce, and pharmacokinetic data for injected supratherapeutic use are limited.
    Aim: To validate a practical liquid chromatography-tandem mass spectrometry (LC-MS/MS) urine assay, estimate optimal detection time-points in clinical settings, and define concentration cut-offs at those time-points.
    Methods: We interviewed people with injecting Tapentadol use for last-use details (time since use, dose). Multiple urine specimens were collected (May 2023-Feb 2024). LC-MS/MS quantification was validated using UNODC guidelines. Optimal thresholds and maximal accuracy were estimated at prespecified clinically relevant time-points (24, 72, 120, and 168 hours).
    Results: We analyzed 778 samples from 342 male patients; median age 24 years (IQR 22-26). Median daily Tapentadol dose 1,000 mg (IQR 500-1500); median injection frequency 10/day (IQR 8-15); median last-use-dose 300 mg (IQR 200-500). Urine concentrations declined exponentially over time. Analytical performance: linearity r² > 0.998 (50-1000 ng/mL), negligible carryover, matrix effect ≤10%, and limit of quantification 1 ng/mL. Accuracy was highest at 72 hours with an optimal concentration cut point of 205 ng/mL (sensitivity 1.00, specificity 0.98, and accuracy 0.99).
    Conclusion: We report a feasible, validated LC-MS/MS urine assay for Tapentadol with good performance at clinically relevant time-points, best performance being at 72 hours after last use. Tapentadol concentration decreased exponentially over time (first-order elimination kinetics), but remained detectable beyond 48 hours, possibly due to saturation kinetics with supratherapeutic-dose IV use or the impact of excipients. These concentration thresholds can support objective monitoring of abstinence/relapse in clinical care.
    Keywords:  Elimination pharmacokinetics; LC–MS/MS; people who inject drugs (PWID); tapentadol; urine drug testing
    DOI:  https://doi.org/10.4103/indianjpsychiatry_945_25
  22. Cancer Treat Res. 2026 ;195 237-247
      Tools for studying cancer metabolism include mass spectrometry (MS) and nuclear magnetic resonance (NMR) spectroscopy for metabolomics, metabolic imaging (PET, MRI, MRS) for in vivo analysis, and metabolic flux analysis (MFA) with stable isotope tracers to track metabolic pathways. Other technologies involve microfluidic systems for simulating tumor environments and fluorescence-activated cell sorting (FACS)-based methods for analyzing immune cell metabolism. Multiple analytical platforms that facilitate the detection of metabolites in cells and living organisms have been utilized to study cancer metabolism. In this section, we will discuss how these techniques have contributed to the study of cancer metabolism and how they have led to advances in our understanding of metabolic reprogramming and biological phenotypes.
    Keywords:  Analytical platforms; Cancer metabolism; Metabolites
    DOI:  https://doi.org/10.1007/978-3-032-21861-2_12
  23. Anal Methods. 2026 May 18.
      Salivary metabolomics is increasingly positioned as a low-burden biochemical layer for athlete monitoring, but its translational value depends less on biomarker novelty alone than on whether the analytical workflow is sufficiently standardized for repeated real-world use. A methods-centered assessment of saliva therefore focuses on how collection control, preprocessing, extraction strategy, separation chemistry, platform selection, normalization, and quality assurance determine interpretability. Current athlete and exercise studies consistently indicate that salivary metabolic profiles respond to acute exercise, repeated competition, and training-related strain, with recurrent signals in amino acids, hydrophilic stress-related metabolites, and broader multimetabolite signatures. However, the literature remains limited by small cohorts, insufficient longitudinal validation, inconsistent sampling states, and incomplete reporting of front-end handling and analytical QA. Comparative reading across NMR, LC-MS, GC-MS, and CE-MS suggests that no single platform is universally optimal: NMR offers strong reproducibility and baseline phenotyping; LC-MS offers broad coverage but requires stronger quantitative discipline; GC-MS remains useful for derivatizable central metabolites; and CE-MS is especially informative for polar and ionic salivary metabolites, although its practical deployment is constrained by reproducibility and alignment challenges. The main translational bottleneck is therefore not whether saliva changes with exercise stress, but whether the workflow can separate biology from pre-analytical and analytical drift. The most credible route toward decision-grade athlete monitoring is a platform-aware workflow that combines standardized passive-drool sampling, explicit preprocessing and extraction logic, repeated within-athlete baselines, targeted or pseudo-targeted validation panels, and multimodal integration with performance and training data.
    DOI:  https://doi.org/10.1039/d6ay00755d
  24. Anal Bioanal Chem. 2026 May 22.
      Human pancreatic islets are highly heterogeneous; thus, understanding their biological organization is crucial for elucidating metabolic function and diabetes pathogenesis. High-resolution mass spectrometry imaging of intact human pancreas is challenging due to the small size and dispersed distribution of individual islets within dense exocrine tissue. Here, we establish an ultra-low-flow-rate DESI mass spectrometry imaging (u-DESI-MSI) platform that enables lipidomic analysis of individual islets in human pancreatic tissue. Optimization of raster step size and scan rate parameters for u-DESI resulted in lipid ion images with enhanced spatial fidelity. The analysis demonstrates a highly reproducible central-peripheral spatial lipid distribution within pancreatic tissue. Diacyl phosphatidylcholines (diacyl-PCs), ether-linked phosphatidylcholines (ether-linked PCs) and sphingomyelins (SMs) are predominantly localized to the central endocrine region and co-register with intact insulin distributions, as further validated by matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI). In contrast, specific lysophosphatidylcholines (LPCs) delineate the endocrine-exocrine interface. These results indicate the existence of position-dependent lipid organization within human islets. This platform provides a robust spatial-mapping foundation for future studies investigating structural and metabolic alterations in human islets under disease conditions.
    Keywords:  Human pancreatic islets; Lipidomic analysis; MALDI-MSI; Mass spectrometry imaging; Spatial distribution; u-DESI-MSI
    DOI:  https://doi.org/10.1007/s00216-026-06557-4
  25. Carbohydr Polym. 2026 Aug 01. pii: S0144-8617(26)00515-1. [Epub ahead of print]385 125398
      Bottom-up analysis of glycopeptides by liquid chromatography-mass spectrometry (LC-MS) plays a critical role in the detection and relative quantification of all glycoforms at each glycosylation site. Reversed-phase (RP) nanoLC-MS in particular is a favored technique for analyzing highly glycosylated proteins due to its sensitivity and accessibility. However, analyzing glycopeptides with large, diverse glycan chains presents challenges such as insufficient and largely varying chromatographic retention. Specifically, hydrophilic glycopeptides consisting of a short, hydrophilic peptide portion with a large, hydrophilic glycan are not retained. We present a RP-nanoLC-MS method that allows for the full characterization of highly hydrophilic glycopeptides. Glycopeptide retention was increased using the amine-reactive and relatively hydrophobic TMTPro Zero label that was covalently attached to all (glyco)peptides. To further increase retention, endoproteinase Lys-C was used to perform proteolysis, generating glycopeptides exhibiting two primary amine groups that were labeled with two TMTPro Zero tags, thereby achieving RP retention of the most hydrophilic glycopeptide analytes. The workflow was applied to two E. coli O-antigen bioconjugates exhibiting highly diverse N-glycopeptides with glycan chains ranging in size between 4 and more than 70 monosaccharides. This optimized approach enables bottom-up analysis of glycoproteins exhibiting large glycans of very high hydrophilicity, supporting comprehensive site-specific glycosylation analysis. HYPOTHESIS: Different glycopeptides with unfavorable chromatographic properties can be detected and characterized using TMTPro Zero labeling and mass spectrometry.
    Keywords:  Glycoconjugate; Glycopeptide analysis; Mass spectrometry; RP-nanoLC-MS; TMTPro Zero
    DOI:  https://doi.org/10.1016/j.carbpol.2026.125398
  26. Rapid Commun Mass Spectrom. 2026 Aug 30. 40(16): e70112
       RATIONALE: Cannabinoids comprise a chemically diverse group of meroterpenoids whose extensive isomerism, variable side-chain length, and frequent oxidative or rearranged derivatives lead to strongly overlapping yet characteristic MS/MS fragmentation patterns. In untargeted LC-MS/MS datasets, this combination of structural diversity and spectral similarity complicates annotation, particularly when reference spectra are sparse or unavailable. Library-based approaches, therefore, recover only a limited fraction of the cannabinoid-related chemical space that is routinely observed in experimental data.
    METHODS: In this work, we apply MassQL to encode established cannabinoid fragmentation chemistry into rule-based queries. The resulting compendium covers major cannabinoid subclasses, including neutral and acidic cannabinoids, varinic analogs (C3 side-chain cannabinoids), and structurally modified derivatives, using combinations of diagnostic fragment ions, neutral loss patterns, adducts, and fragment co-occurrence logic. Importantly, class-level retrieval does not depend on complete or unambiguous precursor m/z information and can be driven solely by MS/MS evidence.
    RESULTS: Application of this framework to a publicly available untargeted LC-MS/MS dataset demonstrates that rule-based querying can recover known cannabinoids while highlighting additional features that share consistent cannabinoid-like fragmentation patterns. These features include putative analogs, transformation products, and derivatized forms that are not represented in current spectral libraries. At the same time, certain known features, such as in-source dehydrated ions, may be under-recovered depending on query design, illustrating current methodological limitations.
    CONCLUSIONS: This study demonstrates the feasibility and interpretability of chemically informed, rule-based MS/MS querying for cannabinoid discovery. Rather than replacing spectral library matching, MassQL-based class-level retrieval provides complementary hypothesis-generating evidence capable of expanding detectable cannabinoid chemical space beyond currently available reference spectra. The results also highlight the importance of polarity-aware fragmentation curation for reliable query-driven metabolomics workflows. MassQL class-level matches should be viewed as chemically informed hypotheses that complement, rather than replace, spectral library identification, while providing a basis for future systematic validation and benchmarking.
    Keywords:  MS/MS fragmentation; MassQL; analog discovery; cannabinoid analysis; neutral loss patterns; rule‐based class‐level retrieval; tandem mass spectrometry
    DOI:  https://doi.org/10.1002/rcm.70112
  27. J Mass Spectrom. 2026 Jun;61(6): e70067
      This research presents a novel approach to accelerate quantitative mass spectrometry imaging (qMSI) measurements using convolutional neural networks (CNNs) with a transfer learning approach. Current methods are time consuming, require numerous specific steps that allow for the introduction of error, and involve meticulous data analysis. The concept is to build a machine learning model that can be used for future qMSI experiments thereby saving time and decreasing variability. In essence, this model is a CNN trained by transfer learning on a smaller dataset of ion images with a known concentration of analyte, which is then applied to future qMSI studies when quantifying the same molecule in the same tissue type. This enhances the speed with which this analysis can be completed and, in theory, decreases the variability seen with previous methods. In this work, we demonstrate that, by using previously collected MSI data and a transfer learning approach, our CNN model allows for the accurate concentration to be determined on new tissues.
    Keywords:  IR‐MALDESI; convolutional neural network; machine learning; quantitative mass spectrometry imaging
    DOI:  https://doi.org/10.1002/jms.70067
  28. Talanta. 2026 May 12. pii: S0039-9140(26)00632-6. [Epub ahead of print]309 129976
      This study presents the development and validation of a highly accurate high-throughput method for the simultaneous determination of 24 representative pesticides in leek samples. The approach integrates a matrix-tailored QuEChERS procedure with complementary low-pressure gas chromatography and ultra-performance liquid chromatography, both coupled to isotope dilution tandem mass spectrometry (LPGC-MS/MS and UHPLC-MS/MS). A systematic investigation of rapid dual-chromatographic separation, sample preparation workflow and hybrid classic/computation-aided calibration strategy was undertaken to maximize analyte recovery and suppress bias. The developed strategy effectively compensated for matrix-induced signal perturbations, reducing matrix effects to within ±20% for GC and ±10% for LC analyses. Comprehensive validation according to SANTE guidelines demonstrated high accuracy (93-111% for GC, 94-105% for LC), sensitivity (LOQ ≤10 μg/kg for most analytes), and precision (RSD <6%). The method's performance was established through its critical applications: i) assigning certified values to a leek matrix reference material with low relative expanded uncertainties (5-10%, k = 2); ii) serving as the reference method in seven proficiency testing schemes to ensure inter-laboratory comparability; and iii) screening 47 commercial leek samples. This survey revealed a 98% pesticide detection frequency and a 51% exceedance rate of EU maximum residue limits, highlighting significant food safety concerns, particularly for pyrethroids and neonicotinoids.
    Keywords:  Food safety; Isotope dilution tandem mass spectrometry; Matrix effect; Multi-class pesticides; Proficiency testing; Reference material value assignment
    DOI:  https://doi.org/10.1016/j.talanta.2026.129976
  29. Bioanalysis. 2026 May 21. 1-6
       AIM: During clinical sample analysis unforeseen problems arose using a previously validated assay for the quantification of diclofenac in the concentration range from 0.0500 to 50.0 ng/mL. Here, we describe the troubleshooting process leading to the identification of the root cause and resulting changes in assay development strategy for robust supported liquid extraction (SLE)-based assays for clinical application.
    METHODS: Individual steps of the sample preparation workflow and subsequent analysis with liquid chromatography and mass spectrometry (LCMS) were examined. Troubleshooting results were tested using stored validation samples and pooled clinical samples for confirmation.
    RESULTS: The root cause for altered assay performance could be identified as the SLE plate batch effect attributable to variability in the sorbent material (diatomaceous earth). Reducing the sample loading volume applied to the SLE plates yielded purer extracts and consistent chromatographic performance. Quantitative recovery and signal consistency were restored after the modification.
    CONCLUSION: Assay robustness was improved by underloading SLE plates. After adjusting the method and re-validation, clinical samples were successfully analyzed. The internal method development strategy was adjusted to avoid full capacity loading of SLE plate with natural sorbents.
    Keywords:  LC-MS/MS; Supported liquid extraction (SLE); diatomaceous earth; diclofenac; troubleshooting
    DOI:  https://doi.org/10.1080/17576180.2026.2677733