bims-metlip Biomed News
on Methods and protocols in metabolomics and lipidomics
Issue of 2026–06–07
forty-five papers selected by
Sofia Costa, Matterworks
  1. Development and Validation of a Rapid LC-MS/MS Method for Carfilzomib Quantification in Plasma from Multiple Myeloma Patients.
  2. Targeted Livestock Metabolomics: A Review of Liquid chromatography-Mass Spectrometry-Based Approaches.
  3. A semi-automatization magnetic solid-phase extraction method of LC-MS/MS for the quantification of homocysteine and its related metabolites in serum.
  4. Comprehensive optimization of chromatographic separation and iterative data acquisition for liquid chromatography-tandem mass spectrometry non-targeted plasma metabolomics: Enhancing feature-based molecular networking.
  5. A simple, high-throughput LC-MS/MS method for the simultaneous quantification of four antiarrhythmic drugs and two metabolites: large-scale application to 622 patient samples.
  6. [Determination of 22 organophosphates and their metabolites and 11 phthalate metabolites in human whole blood by ultra performance liquid chromatography-tandem mass spectrometry].
  7. [Determination of 13 prohibited alkaloids in essential oil-based cosmetics by ultra performance liquid chromatography-tandem mass spectrometry combining QuEChERS purification].
  8. Microwave-Assisted Meta-Chloroperoxybenzoic Acid Epoxidation for Qualitative and Quantitative Analysis of Unsaturated Lipid Double-Bond Positional Isomers by Liquid Chromatography-Tandem Mass Spectrometry.
  9. MetaDilutionR: An R Package for Data-Driven Determination of Optimal Plasma Dilution in Untargeted Metabolomics to Achieve Maximum Metabolite Coverage with ESI Linearity.
  10. Protocol for untargeted lipidomics of human serum using LC-TIMS-PASEF.
  11. Simultaneous determination of trimethylamine N-oxide (TMAO) and its 15 related metabolites by UPLC-MS/MS in human serum.
  12. Ordering molecular diversity in untargeted metabolomics via molecular community networking.
  13. Neutral molecular networks: Polarity-independent tool for mass spectrometry data.
  14. A multiplexed LC-MS/MS assay for comprehensive screening of amino acid metabolism disorders.
  15. IMFrag: A Tool to Recognize In-Source Fragmentation in Ion Mobility-Enabled Data-Independent Acquisition Workflows.
  16. High-Throughput Reactive Desorption Electrospray Ionization Mass Spectrometry for Targeted Derivatization and Analysis of Poorly Ionized Small Molecules.
  17. Exploring Acylcarnitine Metabolism Using Reverse Metabolomics.
  18. Development and validation of a quantitative ultra-performance liquid chromatography quadrupole time-of-flight method for urine organic acid analysis.
  19. [Determination of 16 organic ultraviolet absorbers in drinking water by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry].
  20. A liquid chromatography-mass spectrometry method to quantify total Coenzyme A concentration and isotopic labeling.
  21. Stable isotope labeling LC-MS for profiling the amine submetabolome in a D-lactate treated cell model.
  22. Validation of an HPLC-MS method for simultaneous determination of seven troponin activators in human urine and serum for doping control.
  23. Recent progress in nanomaterial-enhanced SALDI-MSI for spatial metabolomics.
  24. Untargeted microLC-HRMS/MS for Measuring Endogenous Steroids in Mouse Plasma and Human Serum Samples Applied to Studying Polycystic Ovary Syndrome.
  25. Rapid On-Site Analysis of Psychotropic Drugs in Dried Blood Spots by Capillary-in-Capillary Electrospray Ionization (DBS-CC-ESI) Miniature Mass Spectrometry.
  26. LipidCruncher: an open-source platform for processing, visualizing, and analyzing lipidomic data.
  27. Simultaneous Determination of Four Per- and Polyfluoroalkyl Substances (PFAS) in DHA Products using LC-MS/MS for Quality Control and Risk Assessment.
  28. MS-Net: Multi-Similarity-Based Network Annotation for Untargeted Metabolomics.
  29. Extraction and determination of sartans: Recent advances and analytical perspectives.
  30. Metabolite patterns in human urine after oral administration of highly purified Δ8-THCV.
  31. Comprehensive investigation of matrix effect evaluation approaches for reliable quantification in bioanalysis using UHPLC-MS/MS.
  32. [Determination of 40 carbonyl compounds in ambient air by high performance liquid chromatography-triple quadrupole mass spectrometry].
  33. Pseudoenhanced Peak Efficiency in Liquid Chromatography-High Resolution Mass Spectrometry Using Multiple Second Derivatives.
  34. Determination and stereoselective pharmacokinetics of fluralaner enantiomers in broiler chickens by liquid chromatography-tandem mass spectrometry.
  35. Isotope dilution LC-MS/MS for the quantification of ergot alkaloids: a comparative study.
  36. Analytical validation of a dried blood microsampling method to measure androstenedione, 17α‑hydroxyprogesterone, and 11‑ketotestosterone for congenital adrenal hyperplasia monitoring.
  37. Mass spectrometry in laboratory medicine: advances in automation, multiplex biomarker quantification, and diagnostics.
  38. [Determination of seven tire antioxidants and their quinone oxidation products in fine particulate matter by high performance liquid chromatography-tandem mass spectrometry].
  39. Streamlined LC-HRMS-based determination of sterols and triterpenic alcohols in edible oils for authentication purposes.
  40. An Integrated QuEChERS LC-MS/MS Method for Screening, Confirmation, and Quantification of Nitroimidazole Residues in Food.
  41. Translational Quantitative Proteomic Assay for Bacteriophages: A New Frontier in Phage Pharmaceutical Development.
  42. Multi-residue analytical method of 215 pesticides in peanut by GC-Q-Orbitrap MS/MS.
  43. A Polysorbate Structural Atlas Curated from Drift Tube Ion Mobility-Mass Spectrometry Measurements.
  44. An LC-MS-guided AI enabled serum molecule-interpretable SERS platform for exploratory metabolomic analysis in Alzheimer's disease.
  45. Determination of short-chain chlorinated paraffins in marine sediment by automated online solid phase extraction coupled to liquid chromatography-high-resolution mass spectrometry.
  1. J Vis Exp. 2026 May 12.
    Development and Validation of a Rapid LC-MS/MS Method for Carfilzomib Quantification in Plasma from Multiple Myeloma Patients.
    Zhengyan Liang, Jing Qian, Mao Tang, Liya Ye, Zhenhui Jiang, Huanxing Han, Xinran Wang, Xia Tao, Xue Qi, Shouhong Gao.
      Carfilzomib, a second-generation proteasome inhibitor, requires therapeutic drug monitoring (TDM). This study aimed to develop and validate a sensitive and robust liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantification of carfilzomib in human plasma. Plasma samples were processed using protein precipitation with acetonitrile (ACN). Chromatographic separation was achieved on a C18 column (2.1 mm × 100 mm, 3.5 µm) maintained at 40 °C, with a mobile phase composed of ACN and 10 mmol/L ammonium acetate in water (80:20, v/v) delivered at a flow rate of 0.35 mL/min. The method demonstrated excellent linearity over a concentration range of 2.00-1000.00 ng/mL. In addition, high intra-day and inter-day precision and accuracy were observed, with recovery rates for carfilzomib ranging from 84.1%-93.0%. This validated LC-MS/MS method enables accurate, efficient, and sensitive determination of carfilzomib concentrations in plasma from patients with multiple myeloma, thereby supporting the optimization of carfilzomib-based therapy.
    DOI:  https://doi.org/10.3791/70167
  2. J Agric Food Chem. 2026 Jun 02.
    Targeted Livestock Metabolomics: A Review of Liquid chromatography-Mass Spectrometry-Based Approaches.
    Kangkang Xu, Franz Berthiller, Rudolf Krska, Heidi E Schwartz-Zimmermann.
      With the advancement of sophisticated analytical techniques, such as nuclear magnetic resonance spectroscopy and mass spectrometry (MS), metabolomics has become a powerful tool for analyzing and quantifying small molecules in cells, tissues, and biofluids. Among MS-based methods, liquid chromatography-mass spectrometry (LC-MS) is widely used due to its high analyte coverage, sensitivity, and selectivity. Targeted metabolomics quantifies predefined metabolites, in contrast to untargeted approaches that profile all detectable metabolites. This review provides an overview of targeted LC-MS methods and applications in livestock metabolomics, focusing on ruminants and swine, and covering research from the past decade. We discuss sample preparation, LC-MS instrumentation, and method validation, as well as emerging trends including combined LC techniques, integration of targeted and untargeted approaches, and multiomics studies. Current limitations, future directions, and a general workflow for method development are also addressed.
    Keywords:  LC-MS; analytical methods; animal metabolomics; derivatization; dilute and shoot; validation
    DOI:  https://doi.org/10.1021/acs.jafc.5c16870
  3. Pract Lab Med. 2026 Jul;50 e00535
    A semi-automatization magnetic solid-phase extraction method of LC-MS/MS for the quantification of homocysteine and its related metabolites in serum.
    Zhicheng Ye, Xueding Han, Guanfeng Lin, Jianwei Zhou, Yingsong Wu.
       Background: Clinical mass spectrometry is recognized for its high specificity and sensitivity in quantifying small-molecule biomarkers in serum. However, its broad adoption in clinical settings has been limited by challenges such as low automation and time-consuming workflows.
    Methods: This study aimed to develop a rapid, sensitive, and automated magnetic solid-phase extraction(MSPE) method using Hydrophilic-Lipophilic Balance (HLB) magnetic bead-based sample preparation coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous quantification of homocysteine(Hcy) and its related nine metabolites. The method was comprehensively validated for specificity, linearity, sensitivity, accuracy, precision, matrix effects, carry-over; and compared it with solid-phase extraction (SPE) methods.
    Results: Results showed excellent linearity (r2 > 0.995) for all nine biomarkers associated with the homocysteine metabolic cycle. Both the limits of detection and quantification met the clinical requirements. Recoveries at low, medium, and high spiking levels ranged from 85.46% to 114.48%. Intra-day precision (CV) was between 0.82% and 7.63%, and inter-day precision (CV) ranged from 1.62% to 11.43%. Matrix effects were acceptable, with internal standard-normalized matrix factors ranging from 0.83 to 1.19. Carry-over rates were between -7.43% and 5.21%. Method comparison with protein precipitation sample preparation showed correlation coefficients from 0.9462 to 0.9957, indicating no systematic bias.
    Conclusions: In conclusion, the developed semi-automatization method is rapid, highly sensitive, and reproducible, making it suitable for quantitative analysis of these nine homocysteine cycle-related biomarkers in clinical serum samples. It provides a reliable analytical tool for the diagnosis, treatment, and prevention of associated diseases.
    Keywords:  Diagnosis; Homocysteine metabolism cycle; LC-MS/MS; Magnetic solid-phase extraction; Semi-automatization
    DOI:  https://doi.org/10.1016/j.plabm.2026.e00535
  4. J Chromatogr A. 2026 May 27. pii: S0021-9673(26)00457-7. [Epub ahead of print]1783 467128
    Comprehensive optimization of chromatographic separation and iterative data acquisition for liquid chromatography-tandem mass spectrometry non-targeted plasma metabolomics: Enhancing feature-based molecular networking.
    Jiamin Yang, Xiaona Lai, Qing Liu, Yiwen Tao, Hongbo Huang, Bo Ding.
      Liquid chromatography-tandem mass spectrometry (LC-MS/MS) non-targeted plasma metabolomics is essential for biomarker discovery, yet the lack of standardized analytical protocols often compromises data reliability. In this study, we systematically optimized the entire metabolomics workflow, focusing on the integration of feature-based molecular networking (FBMN) to enhance metabolite annotation. Critical parameters, including protein precipitation chemistry, chromatographic selectivity, and data acquisition strategies, were comprehensively assessed. Optimal extraction was achieved using a methanol/ethanol (1:1, v/v) mixture at a 1:4(v/v) sample-to-solvent ratio. For chromatographic separation, an XBridge BEH C18 column outperformed alternatives. Superior peak capacity and ionization efficiency were obtained using 0.1% formic acid (or 10 mM ammonium acetate with 0.1% formic acid) in positive mode, and 10 mM ammonium formate with 0.1% acetic acid in negative mode. While the timing of internal standard addition did not significantly alter the metabolic profile, instrument signal stability became a critical factor for sequences exceeding one week. Notably, the transition to a 100 mm column and the implementation of iterative data-dependent acquisition (DDA) on quality control samples significantly expanded the FBMN size and the number of uniquely annotated compounds. This optimized, robust workflow provides a standardized framework for improving metabolite coverage and annotation confidence in large-scale clinical investigations.
    Keywords:  Chromatographic optimization; FBMN; Iterative acquisition; Non-targeted plasma metabolomics; Protein precipitation
    DOI:  https://doi.org/10.1016/j.chroma.2026.467128
  5. Talanta. 2026 Jun 01. pii: S0039-9140(26)00731-9. [Epub ahead of print]310 130075
    A simple, high-throughput LC-MS/MS method for the simultaneous quantification of four antiarrhythmic drugs and two metabolites: large-scale application to 622 patient samples.
    Hyun-Woo Lee, Mi-Ryung Chun, Seung-Jung Park, Soo-Youn Lee.
      Therapeutic drug monitoring (TDM) of antiarrhythmic drugs (AADs) remains underutilized in clinical practice despite the narrow therapeutic windows and marked inter-individual pharmacokinetic variability of these agents. Here, we developed and validated a simple, high-throughput liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of four commonly prescribed AADs-amiodarone, dronedarone, flecainide, and propafenone-and two metabolites, noramiodarone and debutyldronedarone, in human serum, and applied it to routine clinical samples. Sample preparation consisted of simple protein precipitation using only 10 μL of serum, with a 2 μL injection volume and a total run time of 5.7 min. The method showed excellent linearity for all analytes (R2 > 0.99), acceptable precision (%CV 0.9-5.9%) and accuracy (%bias -6.5-10.5%), minimal matrix effects (88.1-106.6%), satisfactory extraction recoveries (93.9-104.1%), and no significant carryover. No exogenous interference was observed from 25 commonly co-administered cardiovascular drugs, or from 45 neuropsychiatric drugs. The validated assay was successfully applied to 622 serum samples from 524 Korean patients with various arrhythmias. AAD concentrations showed substantial inter-individual variability at identical daily doses, and high proportions of samples were below the therapeutic ranges, supporting the potential utility of routine AAD TDM. This LC-MS/MS method provides a rapid, robust, and clinically practical platform for routine individualized AAD TDM in real-world serum samples with complex matrices.
    Keywords:  Antiarrhythmic drugs; Exogenous interference; LC-MS/MS; Simultaneous quantification; Therapeutic drug monitoring
    DOI:  https://doi.org/10.1016/j.talanta.2026.130075
  6. Se Pu. 2026 Jun;44(6): 682-693
    [Determination of 22 organophosphates and their metabolites and 11 phthalate metabolites in human whole blood by ultra performance liquid chromatography-tandem mass spectrometry].
    Fei-Yun Shi, Hao-Yu Xu, Jun-Hong Li, Meng-Yuan Xu.
      Organic phosphate esters （OPEs） and phthalate esters （PAEs） are two classes of synthetic compounds widely incorporated into various industrial and consumer products as flame retardants and plasticizers. Both exhibit multi-organ cumulative toxicity. In this study， an ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method was developed for the determination of 22 OPEs and their diester metabolites （mOPEs） and 11 phthalate ester metabolites （mPAEs） in whole blood. The whole blood samples were extracted with 0.1% formic acid-acetonitrile by liquid-liquid extraction for protein precipitation， and then purified by HMR S-micro BIO 96-well solid phase extraction column. The filtrate was blown to near dryness with nitrogen， and reconstituted with 0.1% formic acid-acetonitrile solution. The target compounds were detected by UPLC-MS/MS. A Ghost Trap DS-HP chromatographic column （30 mm×2.1 mm） was used as the background ghost peak trap column， and an ACQUITY UPLC® BEH C18 chromatographic column （150 mm×2.1 mm， 1.7 μm） was used as the analytical column. Methanol and 0.5 mmol/L ammonium acetate were used as mobile phase for gradient elution. Electrospray ionization （ESI） was used for MS detection， with both positive and negative ion scanning in the multiple reaction monitoring （MRM） mode. Isotope internal standard method was used for quantification. The results showed that 33 target compounds could be separated within 15 min， and good linear relationships were observed for all target compounds across their respective mass concentration ranges （r=0.993 3-0.999 8）. The limits of detection were 0.003-0.31 ng/mL and the limits of quantification were 0.01-1.02 ng/mL. The spiked recoveries of 33 targets in whole blood samples ranged from 60.5% to 138.3%， with relative standard deviations （RSDs） from 1.6% to 11.0%. The detection rates of tris-（2-chloroisopropyl）phosphate （TCiPP）， triphenyl phosphate （TPHP）， 2-ethylhexyl diphenyl （EHDPP）， mono（2-ethyl-5-hydroxyhexyl） phthalate （MEHHP）， mono-n-butyl phthalate （MNBP） and mono-n-octyl phthalate （MOP） were 100% in 14 whole blood samples， and the highest detection amount of TPHP was 10.04 ng/mL. The developed method is simple to operate， sensitive， accurate， requires small sample volumes， and is cost-effective on reagents. It is suitable for human biomonitoring， and provides a theoretical basis for monitoring organic phosphate and phthalic ester substances in the population.
    Keywords:  organic phosphate esters; phthalate ester metabolites; ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）; whole blood
    DOI:  https://doi.org/10.3724/SP.J.1123.2025.09019
  7. Se Pu. 2026 Jun;44(6): 667-674
    [Determination of 13 prohibited alkaloids in essential oil-based cosmetics by ultra performance liquid chromatography-tandem mass spectrometry combining QuEChERS purification].
    Zhen Liu, Yu-Mei Wang, Jian-Bin Pan, Ling-Li Zong, Yu-Han Song, Xiao-Jie Sun, Hong-Yuan Chen.
      Alkaloids represent a class of naturally-occurring nitrogen-containing compounds widely distributed across diverse plant species. Owing to their well-documented potential to induce adverse effects on human health， certain alkaloids are explicitly prohibited from being used in cosmetic formulations. The escalating global popularity of essential oil-based cosmetics， which commonly incorporate complex botanical extracts， presents a potential avenue for the inadvertent introduction of these prohibited substances. Consequently， the development of robust， sensitive， and efficient analytical methods for their monitoring is of utmost significance for consumer safety and regulatory compliance. This study devises a reliable， high-throughput approach for the simultaneous determination of 13 prohibited alkaloids in essential oil-based cosmetics. It integrates optimized QuEChERS sample preparation with ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. The sample preparation procedure was meticulously designed to maximize efficiency and minimize analyte loss. Chromatographic separation was accomplished on a Waters ACQUITY UPLC HSS T3 column （100 mm × 2.1 mm， 1.8 μm） maintained at a constant temperature of 30 ℃. The mobile phase was composed of （A） acetonitrile and （B） 0.1% （volume fraction） formic acid aqueous solution. A gradient elution program was implemented at a stable flow rate of 0.3 mL/min according to the following profile： an initial 5， a linear increase to 15 （0-2 min）， a rapid rise to 70 （2-4.5 min）， followed by an immediate reversion to the initial 5 （4.5-5.5 min）， which was maintained for re-equilibration until 7.0 min. The injection volume was 5 µL. Detection and quantification were conducted using a triple quadrupole mass spectrometer equipped with an electrospray ionization （ESI） source operating in positive ion mode （ESI+）. Data acquisition was carried out in the multiple reaction monitoring （MRM） mode to ensure superior specificity and sensitivity. For each of the 13 alkaloids， two specific ion transitions were monitored： one for quantitative analysis and the other for confirmatory identification. The method was rigorously validated in accordance with accepted analytical guidelines. All 13 target alkaloids displayed excellent linearity within a mass concentration range of 0.2 to 50 ng/mL， with correlation coefficients （R2） consistently exceeding 0.99. The limits of detection （LODs） and limits of quantification （LOQs）， determined with acceptable accuracy and precision， ranged from 1 µg/kg to 4 µg/kg and 2 µg/kg to 10 µg/kg， respectively. Method accuracy and precision were assessed through recovery tests at three spiking levels， with six replicates at each level. The mean recoveries for all analytes ranged from 83.9% to 119.1%， with associated relative standard deviations （RSDs） all being ≤7.3%， validating the method's high reliability and repeatability. Systematic evaluation indicated that the matrix effects for the 13 analytes were negligible； hence， the solvent calibration curve was adopted for quantitative analysis. The practical applicability of the validated method was demonstrated through the analysis of 50 batches of commercially available essential oil-based cosmetics. This market survey encompassed 15 products specifically marketed for infants or children and 35 products intended for adult use. As a result， none of the 13 target prohibited alkaloids were detected in any of the tested samples above their respective LOQs. A particularly notable accomplishment of this work is the successful development of a sensitive and reliable quantification strategy for oleandrin， a potent cardiotoxic alkaloid for which standardized detection methods in complex cosmetic matrices such as essential oils have been conspicuously absent. In conclusion， this study successfully establishes a simple， rapid， sensitive， and robust QuEChERS-UPLC-MS/MS method. It is comprehensively validated and clearly well-suited for the routine screening， risk monitoring， and quality control of 13 prohibited alkaloids in a wide array of essential oil-based cosmetics. The method offers reliable technical support for regulatory bodies to enforce safety standards and for manufacturers to ensure the safety and compliance of their products， thereby effectively contributing to the protection of consumer health.
    Keywords:  QuEChERS purification; essential oil-based cosmetics; prohibited alkaloids; ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）
    DOI:  https://doi.org/10.3724/SP.J.1123.2025.10009
  8. J Sep Sci. 2026 Jun;49(6): e70460
    Microwave-Assisted Meta-Chloroperoxybenzoic Acid Epoxidation for Qualitative and Quantitative Analysis of Unsaturated Lipid Double-Bond Positional Isomers by Liquid Chromatography-Tandem Mass Spectrometry.
    Danyang Liu, Hongjin Chen, Yong Huang, Ting Zhou.
      Unsaturated lipid double-bond (C═C) positional isomers are closely related to lipid structure and biological function, but their reliable qualitative and quantitative analysis remains challenging by conventional liquid chromatography-mass spectrometry (LC-MS) methods. In this study, we developed a microwave-assisted meta-chloroperoxybenzoic acid (m-CPBA) epoxidation method coupled with LC-tandem MS for the identification and quantification of unsaturated lipid C═C positional isomers. The reaction conditions were optimized to facilitate the formation of fully epoxidized products, simplify the chromatographic peak profiles, and enhance their suitability for targeted quantitative analysis. The developed method showed good analytical performance, including satisfactory linearity (r2 > 0.99), precision (relative standard deviation <15%), recovery (75.5%-106.5%), and acceptable matrix effects (86.0%-117.3%). The method was successfully applied to rat brain tissue and plasma samples from a rat depression model, enabling the quantification of multiple unsaturated lipids and the characterization of their C═C positional isomers in complex biological matrices. These results demonstrate that microwave-assisted m-CPBA epoxidation provides a rapid, efficient, and practical strategy for LC-MS-based analysis of unsaturated lipid isomers.
    Keywords:  biological matrices; derivatization; diagnostic fragmentation; fatty acids; phospholipids
    DOI:  https://doi.org/10.1002/jssc.70460
  9. J Am Soc Mass Spectrom. 2026 Jun 03.
    MetaDilutionR: An R Package for Data-Driven Determination of Optimal Plasma Dilution in Untargeted Metabolomics to Achieve Maximum Metabolite Coverage with ESI Linearity.
    Keerthana Vinod Kumar, Aviral Singh, Sneha Rana, Rakesh Sahay, Pramod P Wangikar.
      High-resolution mass spectrometry (HRMS) instruments for untargeted metabolomics typically offer a linear dynamic range spanning approximately 4 orders of magnitude. However, biological samples contain metabolites spanning concentration ranges far exceeding this window, making dilution optimization critical for reliable quantification. Despite its importance, dilution selection in untargeted workflows is rarely standardized and is often determined empirically through manual inspection, leading to operation outside the linear dynamic range, ion suppression, and compromised reproducibility. To address this, we present MetaDilutionR, an open-source R package that standardizes dilution optimization by systematically evaluating electrospray ionization (ESI) linearity using plasma as a model. MetaDilutionR automates dilution assessments, applying user-adjustable slope and R2 thresholds to classify features as linear or nonlinear and executes the complete analysis via a single function call, ensuring algorithmic reproducibility across users and platforms. The package generates comprehensive outputs, including log2-transformed data, a summary of linear features with their optimal dilution ranges, nonlinear features highlighting potential ion suppression or detector saturation, detailed evaluations across dilution scenarios, and visual regression plot reports. Benchmarking against three established metabolomics workflows demonstrated that the R2-slope criterion of MetaDilutionR reduces false-positive linear assignments. Cross-platform applicability of the algorithm on an independent GC-MS data set confirmed consistent classification performance beyond LC-HRMS. By facilitating systematic identification of metabolite-specific optimal dilution conditions, MetaDilutionR enables metabolites to be quantified within their linear dynamic range─a prerequisite for reliable quantification─thereby enhancing reproducibility and consistency of downstream validation, making it readily integrable into existing metabolomics workflows.
    Keywords:  linearity; metabolite coverage; serial dilution; untargeted metabolomics
    DOI:  https://doi.org/10.1021/jasms.5c00419
  10. STAR Protoc. 2026 Jun 01. pii: S2666-1667(26)00260-1. [Epub ahead of print]7(2): 104607
    Protocol for untargeted lipidomics of human serum using LC-TIMS-PASEF.
    Fernanda Sousa Monteiro, Adriana Zardini Buzatto.
      Here, we present a protocol for untargeted lipidomics of human serum. We describe steps for project design, sample preparation, and reversed-phase liquid chromatography coupled with trapped ion mobility spectrometry and parallel accumulation serial fragmentation (LC-TIMS-PASEF). We then detail procedures for quality control and data processing. The protocol enables comprehensive lipid profiling from 5 μL of serum, yielding annotations across glycerophospholipids, glycerolipids, sphingolipids, sterols, and fatty acyls. The resulting datasets support statistical analysis and integration with complementary omics approaches.
    Keywords:  Mass Spectrometry; Metabolomics; Protocols in Metabolomics and Lipidomics
    DOI:  https://doi.org/10.1016/j.xpro.2026.104607
  11. J Chromatogr B Analyt Technol Biomed Life Sci. 2026 Jun 01. pii: S1570-0232(26)00256-4. [Epub ahead of print]1281 125167
    Simultaneous determination of trimethylamine N-oxide (TMAO) and its 15 related metabolites by UPLC-MS/MS in human serum.
    Shiguang Zhou, Jie Liu, Xia Zhao, Xiaohui Li, Ziwen An, Weitao Su, Jianxin Ma, Yibing Yang, Shuo Wang, Ang Li, Liu Liu.
      Trimethylamine N-oxide (TMAO) is increasingly recognized for its role in the pathogenesis and progression of cardiovascular and metabolic diseases by disturbing fatty acid metabolism. Concurrently, the acylcarnitine profile serves as a critical indicator of associated mitochondrial dysfunction. However, present ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) methodologies often focus on a few targets such as betaine, choline, TMAO, and trimethylamine and lack the integrated capability to monitor simultaneous changes in the acylcarnitine profile. This analytical gap restricts the depth of toxicological investigations into the effects of environmental pollutants as well as the thorough assessment of metabolic homeostasis. In this study, an optimized UPLC-MS/MS method was developed for the simultaneous measurement of TMAO and its 15 related metabolites in human serum. Serum samples underwent pretreatment through targeted ethyl bromoacetate-derivatization and protein precipitation. Using 4% bovine serum albumin as a surrogate matrix, matrix-matched calibration was performed to reduce matrix effects and ensure analytical accuracy. Using 10 mmol/L ammonium formate (pH 4.0) and acetonitrile containing 0.1% formic acid as mobile phases, chromatographic separation was achieved on a HILIC column within a 5.5 min runtime. Positive electrospray ionization and multiple reaction monitoring mode were used to monitor the target analytes. The assay demonstrated good linearity (R2 > 0.992) with limits of detection ranging from 0.012 to 5.2 μg/L. Spike recoveries in real samples were 84.5%-114.9%, with relative standard deviations below 10%. In conclusion, this study presents a rapid and validated UPLC-MS/MS method for simultaneous profiling of a targeted panel of TMAO, its precursors, and functionally related acylcarnitines in human serum. It may support studies investigating their associations with cardiometabolic disorders, chronic kidney disease, and metabolic dysfunction linked to gut microbial metabolism.
    Keywords:  Acylcarnitines; Human serum; TMAO; Trimethylamine; UPLC-MS/MS
    DOI:  https://doi.org/10.1016/j.jchromb.2026.125167
  12. Cell Rep Methods. 2026 Jun 02. pii: S2667-2375(26)00168-2. [Epub ahead of print] 101468
    Ordering molecular diversity in untargeted metabolomics via molecular community networking.
    Elizabeth A Coler, Alexey Melnik, Ali Lotfi, Dana Moradi, Ben Ahiadu, Paulo Wender Portal Gomes, Abubaker Patan, Vincent Charron-Lamoureux, Pieter C Dorrestein, Stephen Barnes, Vladimir Boginski, Alexander Semenov, Alexander A Aksenov.
      Molecules in living systems are not random but are shaped by biological necessity. Mass spectrometry (MS) is a powerful tool for exploring these complex molecular landscapes. Molecular networking links metabolites by spectral similarity, but conventional methods leave many nodes disconnected. We introduce molecular community networking (MCN), which identifies natural molecular clusters and prunes them to keep the strongest links. The approach increases connectivity to about 95% of molecules and better captures structurally related compounds, including distinct ion forms and in-source fragmentation ions. MCN also improves the mapping of molecular space, helping distinguish true novel molecules from artifacts. Using MCN, we discovered dipeptide-conjugated bile acids associated with Bifidobacterium breve and proposed structures for previously unexplored N-acyl amides that interact with G protein-coupled receptors. We also built a global metabolome map from public GNPS/MassIVE data, covering about 8.4 million molecular features, creating a "roadmap" for molecular diversity.
    Keywords:  CP: computational biology; CP: metabolism; gas chromatography-mass spectrometry; liquid chromatography-mass spectrometry; metabolomics; molecular community networking; molecular networking
    DOI:  https://doi.org/10.1016/j.crmeth.2026.101468
  13. Anal Chim Acta. 2026 Sep 15. pii: S0003-2670(26)00658-6. [Epub ahead of print]1415 345708
    Neutral molecular networks: Polarity-independent tool for mass spectrometry data.
    Nicola Dalla Valle, Pietro Franceschi, Mar Garcia-Aloy, Peter Robatscher, Sabine Oettl, Michael Oberhuber.
      Untargeted mass spectrometry-based metabolomics generates large-scale fragmentation data, typically analyzed separately in positive and negative ionization modes. The fragmentation patterns of the same molecule usually capture distinct but complementary structural information across polarities. Evaluating them simultaneously, rather than in separate molecular networks, can enhance the overall informativeness and speed the analysis. In this paper, we introduce the Neutral Molecular Network (NMN) concept, a novel strategy that unifies complementary fragmentation patterns from both polarities into a single "neutral pseudo-spectra". NMNs outperformed polarity-specific networks on several large-scale publicly available MS/MS libraries in terms of chemical reliability of spectral matches and clustering capability. The improved performances were further confirmed through the analysis of a biological untargeted dataset of Alternaria fungal extracts, where this approach facilitated the identification of previously uncharacterized toxin derivatives. NMN offers a polarity-independent framework for the structural interpretation of untargeted MS/MS data. This method can improve the efficiency of metabolite annotation pipelines and can be applicable to diverse metabolomics workflows.
    Keywords:  Alternaria; Electrospray ionization; Mass spectrometry; Molecular network; Untargeted metabolomics
    DOI:  https://doi.org/10.1016/j.aca.2026.345708
  14. Talanta Open. 2025 Dec;12 100523
    A multiplexed LC-MS/MS assay for comprehensive screening of amino acid metabolism disorders.
    Jisha Chandran, Madan Gopal Ramarajan, Vykuntaraju Kammasandra Nanjundagowda, Aruna Gowdra, Jayesh Warade, Anikha Bellad, Kannan Rangiah.
      Advancements in liquid chromatography-tandem mass spectrometry (LC-MS/MS) are redefining the landscape of clinical diagnostics, particularly in the context of newborn screening for inborn errors of metabolism. Conventional analytical platforms are often limited by a small number of analytes and require multiple platforms for subsequent analyses, thereby impacting timely diagnosis and management. This study describes the development of a multiplexed targeted mass spectrometry-based assay for simultaneous detection and quantitation of amines, including amino acids and their derivatives, from plasma, urine and dried blood spots. The method utilizes a single step derivatization strategy based on one step click chemistry that simplifies sample preparation while improving analytical sensitivity allowing for detection of analytes at sub-picomolar concentrations. Furthermore, we adopted a strategy of generating heavy isotopically labeled standards by chemically modifying the corresponding light standards using a stable isotope labeled derivatizing agent, enabling their use as internal standards for quantification. This approach can offer a cost-effective and scalable solution for the early detection and management of inherited metabolic disorders, particularly in cases where accurate detection of amines is critical.
    Keywords:  Amines; Amino acid; Inborn errors of metabolism; LC-MS; Newborn Screening; Quantification
    DOI:  https://doi.org/10.1016/j.talo.2025.100523
  15. Anal Chem. 2026 Jun 06.
    IMFrag: A Tool to Recognize In-Source Fragmentation in Ion Mobility-Enabled Data-Independent Acquisition Workflows.
    Ryan Nguyen, Anvitaa Anandkumar, Griffin Rangel, Jennifer Liem, Yvonne S Lin, Libin Xu.
      High-resolution mass spectrometry is a powerful tool for untargeted analysis. However, in-source fragmentation (ISF) could lead to the misidentification of compounds in untargeted metabolomics or exposomics studies. To prevent misidentification and to strengthen compound identification through MS/MS spectral library matching, we developed IMFrag, a Jupyter notebook-based tool that utilizes structural information gained from ion mobility-mass spectrometry (IM-MS) as an orthogonal technique to differentiate independent precursor ions from fragments formed via ISF. We first examined l-tryptophan, which is an essential amino acid that undergoes extensive fragmentation during electrospray ionization (ESI). IM-enabled data-independent acquisition (IM-DIA) analysis revealed distinct mobility signatures for identical fragment ions formed at different instrument sites, enabling discrimination between ISFs generated prior to the IM drift tube and fragments produced via postmobility collision-induced dissociation. Similar patterns were observed for a structurally diverse collection of small molecules. Additional structural information could also be inferred from the IM-DIA workflow, such as unique dimers, protonation sites, and distinct ion types that were not apparent from LC-MS alone. These insights were shown to be useful when applied to healthy human plasma samples, which served as a more complex and biologically relevant matrix that contained ambiguities, such as coeluting, isobaric candidate structures. Thus, IMFrag was developed as an accessible framework for interrogating MS1 and post-IM MS2 chemical features in untargeted data sets and can be integrated into untargeted analysis pipelines or used to support the development of ISF-derived MS/MS spectral libraries.
    DOI:  https://doi.org/10.1021/acs.analchem.6c01388
  16. Anal Chem. 2026 Jun 01.
    High-Throughput Reactive Desorption Electrospray Ionization Mass Spectrometry for Targeted Derivatization and Analysis of Poorly Ionized Small Molecules.
    Yunfei Feng, Kitmin Chen, Kai-Hung Huang, Joseph V Caruso, Christopher J Welch, R Graham Cooks, Christina R Ferreira, Nicolás M Morato.
      Mass spectrometry (MS) analysis of some biologically relevant compounds is limited because of their inherently poor ionization efficiency. This challenge can often be overcome by incorporating easily ionized moieties via functional-group-targeted chemical derivatization. However, the wide variety of derivatization agents and conditions can make method development cumbersome. In this study, we employ an automated high-throughput (HT) platform based on desorption electrospray ionization (DESI) MS to rapidly screen (1 sample per second) and select appropriate derivatization strategies for poorly ionized analytes leveraging accelerated on-the-fly microdroplet reactions. This approach allowed the rapid identification of efficient derivatization strategies that were then readily applied to the qualitative and quantitative analyses of molecules of biological importance. Specifically, hydroxysteroids (e.g., cholesterol, testosterone, and cholecalciferol) were imaged in tissue sections using 4-formyl-1-methylpyridinium benzenesulfonate without the loss of the intrinsic spatial resolution of DESI, while 4-borono-N,N,N-trimethylbenzenaminium allowed sensitive and HT quantitation of urinary 3-methoxy-4-hydroxyphenylglycol, a metabolite whose urine levels have been correlated with neurological disorders.
    DOI:  https://doi.org/10.1021/acs.analchem.6c00291
  17. Anal Chem. 2026 Jun 04.
    Exploring Acylcarnitine Metabolism Using Reverse Metabolomics.
    Allison J Keys, Daniel J Wiener, Sara M Pacini, Chengze Sun, Lindsay E Sandusky, Huaiyang Zhong, Emily C Gentry.
      Untargeted mass spectrometry (MS) is a valuable tool for studying human metabolism and identifying small molecule disease biomarkers. However, annotation of chemical structures and validation of findings across numerous cohorts remains challenging. Reverse metabolomics employs a structure-driven approach to overcome these issues by searching spectra of known structures against an entire repository of untargeted LC-MS/MS data to see where metabolites of interest are found. This work uses reverse metabolomics to study acylcarnitine (AC) metabolism in humans and other animals. Here, a library of 76 ACs was chemically synthesized then searched against public metabolomics data to explore where metabolites of interest are detected. From this analysis, it was determined that acylcarnitines are most frequently observed in human and mouse samples, with about 90% of all searched AC structures present in both blood and fecal samples from these species. This work identified positive associations between certain AC structures and disease, indicating their capacity as health biomarkers. Machine learning was applied, determining that AC presence and absence data can accurately predict healthy versus unhealthy individuals with good precision and recall, albeit the models lack disease specificity. Overall, our findings suggest that AC profiles can serve as valuable biomarkers for disease detection throughout the entire lifespan and should be examined for their potential beyond current clinical screening protocols.
    DOI:  https://doi.org/10.1021/acs.analchem.6c01418
  18. Am J Clin Pathol. 2026 Jun 04. pii: aqag061. [Epub ahead of print]165(6):
    Development and validation of a quantitative ultra-performance liquid chromatography quadrupole time-of-flight method for urine organic acid analysis.
    Yi Xiao, Michael Wakefield, Mari Ishak Gabra, Lidong Zhai, Edward Ki Yun Leung.
       OBJECTIVES: Urine organic acid analysis is essential for diagnosing inborn errors of metabolism and is conventionally performed using multistep, labor-intensive sample preparation and gas chromatography-mass spectrometry (GC-MS). We sought to develop and validate a quantitative ultra-performance liquid chromatography quadrupole time-of-flight (UPLC-QTOF) method with a "dilute-and-shoot" approach.
    METHODS: 20 µL of calibrator, quality control material, or urine specimen, normalized by creatinine concentration, was mixed with mobile phase A (0.05% formic acid in water) and internal standards to a final volume of 440 µL. The supernatant was injected onto a Waters ACUITY Premier HSS T3 UPLC column, with data acquired in MSE mode on a Waters Xevo G3 QTOF mass spectrometer and quantification achieved using both linear and quadratic regressions.
    RESULTS: The method quantifies 27 analytes and separates diagnostically important isomers in 20 minutes. Repeatability and reproducibility were 12% or less coefficient of variation, with no carryover observed. Spike-recovery studies demonstrated recoveries between 85% and 115%, and concordant results were obtained from 51 urine specimens vs the conventional GC-MS method. No matrix effect was identified except for 3-hydroxyglutaric acid. Compared with other UPLC-QTOF methods, improved chromatographic performance was achieved with the Premier HSS T3 column, while MSE high-resolution MS data provided fragmentation information to support higher-confidence compound identification. Compared with conventional GC-MS methods, this method requires substantially lower specimen volume and simplified sample preparation.
    CONCLUSIONS: This UPLC-QTOF dilute-and-shoot urine organic acid method demonstrated acceptable analytical and clinical performance. Continued optimization will be pursued to expand the panel and support the diagnosis of a broader range of inborn errors of metabolism.
    Keywords:  UPLC-QTOF; clinical mass spectrometry; high-resolution mass spectrometry; inborn errors of metabolism; mass spectrometry validation; urine organic acid
    DOI:  https://doi.org/10.1093/ajcp/aqag061
  19. Se Pu. 2026 Jun;44(6): 650-657
    [Determination of 16 organic ultraviolet absorbers in drinking water by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry].
    Zhuo Wang, Can Zhao, Bi-Xiong Ye, Yong-Yan Chen.
      Organic ultraviolet absorbers （OUVAs） are a class of emerging contaminants that have garnered significant attention in recent years. In response to the characteristics of high detection frequency and low concentrations of OUVAs in water bodies， this study established an analytical method based on solid phase extraction （SPE） coupled with ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） for the simultaneous determination of 16 OUVAs （nine UV stabilizers and seven UV filters） in drinking water. The 500 mL water sample was pretreated with 25 mg ascorbic acid， acidified to pH 2-3， and spiked with 1 mL of 5 μg/L mixed internal standard working solution. Target compounds were enriched and concentrated using an HLB solid phase extraction cartridge （200 mg/6 mL）. Separation was achieved on an Acquity Premier BEH C18 column （100 mm×2.1 mm， 1.7 μm） using a gradient elution with methanol and 2 mmol/L ammonium acetate aqueous solution as the mobile phases. Detection was performed using electrospray ionization in positive mode and multiple reaction monitoring （MRM）， with quantification carried out by the internal standard method. The precision and accuracy of the established method were evaluated using drinking water as the matrix. The results showed that all 16 OUVAs exhibited good linearity within their respective mass concentration ranges， with correlation coefficients （r） greater than 0.992. The method detection limits （MDL， S/N=3） were 0.03-5 ng/L， and the method quantification limits （MQL， S/N=10） were 0.1-15 ng/L. At spiked levels of 5， 20 and 50 ng/L， the recoveries of the target analytes ranged from 75.0% to 130.6%， with relative standard deviations （RSDs） ranging from 0.9% to 12.9% （n=6）. A total of seven source water samples and seven drinking water samples were analyzed using this method. The results showed that two OUVAs， 2-hydroxy-4-methoxybenzophenone （UV-9） and octocrylene （OC） were detected. In source water， the mass concentrations of UV-9 ranged from <MQL to 13.4 ng/L， while OC mass concentrations ranged from 5.0 to 32.23 ng/L. In drinking water， UV-9 was detected at 0.4 ng/L， and OC mass concentrations ranged from <MQL to 13.2 ng/L. This method is suitable for the trace analysis of 16 OUVAs in drinking water， demonstrating good accuracy and precision. It effectively improves the detection efficiency of OUVAs in water and can be used for the environmental monitoring and analysis of OUVAs in drinking water in China.
    Keywords:  drinking water; organic ultraviolet absorbers （OUVAs）; solid phase extraction （SPE）; ultra-high performance liquid chromatography-triple quadrupole mass spectrometry （UHPLC-MS/MS）
    DOI:  https://doi.org/10.3724/SP.J.1123.2025.10015
  20. bioRxiv. 2026 May 20. pii: 2026.05.19.726225. [Epub ahead of print]
    A liquid chromatography-mass spectrometry method to quantify total Coenzyme A concentration and isotopic labeling.
    Amelia L Taylor, Nathaniel W Snyder, Caroline R Bartman.
      Coenzyme A is an essential cofactor synthesized from pantothenate, cysteine, and ATP, and is involved in numerous processes of cellular metabolism through its ability to carry activated acyl groups. Coenzyme A participates in catabolism of carbohydrate, fat and amino acids; biosynthesis of fatty acids, cholesterol and heme; and protein modification including acetylation and 4-phosphopantetheinylation. Despite CoA's critical functions, the regulation of CoA levels and the rate of CoA synthesis in different cell types and disease states are not well understood. One reason for this gap is that many acyl-CoA species are analytically challenging to measure due to factors including instability, poor ionization, and the wide range of biochemical properties conferred by different acyl chain lengths. In addition, most current methods do not support analysis of CoA isotopic labeling, which is required to quantify CoA synthesis rate or to measure absolute concentration using isotope-labeled internal standards. Here, we describe a method to quantify the concentration and isotopic labeling of total CoA, defined as the sum of CoASH plus all acyl-CoA species. Acyl-CoA species are hydrolyzed using sodium hydroxide to remove acyl chains, then CoA is derivatized on the thiol with N-ethylmaleimide (NEM). Following protein precipitation and solid phase extraction, samples are analyzed by liquid chromatography-mass spectrometry. This method is linear in a wide range that captures mouse tissue CoA levels, with accuracy within 15% error and precision below 15% relative standard deviation for both pure standards and tissue samples. We applied this method to measure total CoA concentration in five tissues from male and female mice, and total CoA synthesis rate in mouse liver via infusion of 13 C- 15 N-pantothenate. Overall, this method offers a tractable approach to measure total CoA concentration and isotopic labeling to enable study of total CoA synthesis rates and concentrations in health and disease.
    DOI:  https://doi.org/10.64898/2026.05.19.726225
  21. Anal Chim Acta. 2026 Aug 22. pii: S0003-2670(26)00599-4. [Epub ahead of print]1412 345649
    Stable isotope labeling LC-MS for profiling the amine submetabolome in a D-lactate treated cell model.
    Yue-Qiang Chen, Xiao-Xia Dong, Li Liu, Xiu-Ping Chen, Chen-Guo Feng, Li-Xing Zhan, Yue Su, Fang Zhang, Yin-Long Guo.
       BACKGROUND: Alterations in the amine submetabolome are closely associated with cellular metabolic status and are important for understanding metabolic regulation under intervention conditions. In this study, a stable isotope labeling derivatization combined with liquid chromatography-mass spectrometry (LC-MS) was employed to characterize alterations in the cellular amine submetabolome. Optimization of chromatographic separation and cellular metabolic quenching procedures improved the separation performance of amine metabolites while enabling more accurate preservation of the metabolic state at the time of sampling.
    RESULTS: The established method was applied to a D-lactate treated BEAS-2B cell model to evaluate amine submetabolome alterations under different compound intervention conditions. The results demonstrated that selenomethionine (SeMet) and berberine alleviated D-lactate induced abnormalities in the amine submetabolome and showed metabolic regulatory effects consistent with tumor-suppressive trends observed under in vivo experiments.
    SIGNIFICANCE: Overall, this analytical strategy enables characterization of the amine submetabolome in complex biological samples and provides a reliable methodological reference for metabolome-based investigations of cellular metabolic alterations.
    Keywords:  Amine submetabolome; BEAS-2B cells; D-lactate; LC–MS; Lung cancer; Stable isotope labeling
    DOI:  https://doi.org/10.1016/j.aca.2026.345649
  22. J Chromatogr B Analyt Technol Biomed Life Sci. 2026 May 29. pii: S1570-0232(26)00236-9. [Epub ahead of print]1281 125147
    Validation of an HPLC-MS method for simultaneous determination of seven troponin activators in human urine and serum for doping control.
    Mingxue Yang, Xiaoyun Zhang, Lili Xing, Xiaochen Huang, Yunda Li, Haishui Shi, Guojun Li, Kaoqi Lian.
      Troponin activators have been classified as S0 (non-approved substances) by the World Anti-Doping Agency (WADA) since 2024. A rapid, sensitive, and reliable high-performance liquid chromatography-mass spectrometry (HPLC-MS) method was developed for the determination of seven troponin activators (GSK854, Nelutroctiv, Tirasemtiv, RPI-194, EMD57033, 3-chlorodiphenylamine, Reldesemtiv) in urine and serum. For urine samples, liquid-liquid extraction (LLE) was used for pretreatment. The method demonstrated limits of detection (LODs) of 0.04-0.36 ng/mL, with accuracy ranging from 80.7 to 114.5% and precision with RSDs below 14.6% for all analytes. The concentrations of the analytes remained within approximately 3.0-4.5 ng/mL over 7 days under various storage conditions, indicating generally acceptable stability, although compound-dependent degradation was observed, particularly for 3-chlorodiphenylamine. For serum samples, pretreatment combined acetonitrile precipitation and QuEChERS. The LOD was 0.007-0.52 ng/mL, with accuracy ranging from 74.0 to 118.5% and precision (RSD) below 12.1%, and good linearity in the calibration range. This method is expected to contribute significantly to anti-doping control.
    Keywords:  Anti-doping; HPLC-MS; Troponin activators; Urine and serum testing
    DOI:  https://doi.org/10.1016/j.jchromb.2026.125147
  23. Anal Bioanal Chem. 2026 Jun 05.
    Recent progress in nanomaterial-enhanced SALDI-MSI for spatial metabolomics.
    Xingyue Liu, Jinyang Wang, Qinpei Wei, Zhifeng Chen, Qiulei Lang, Guolin Li, Wei Duan.
      Spatial metabolomics enables in situ mapping of metabolites within tissues, which is crucial for understanding physiological and pathological processes, including tumor metabolic reprogramming, neurodegenerative disease mechanisms, and drug distribution in target organs. Mass spectrometry imaging is a powerful tool for spatial metabolomics research. With the advancement of mass spectrometry and nanotechnology, surface-assisted laser desorption/ionization mass spectrometry imaging (SALDI-MSI) that uses nanomaterials instead of organic matrices has emerged, effectively overcoming the inherent limitations of traditional methods in small-molecule metabolite analysis, such as matrix background interference and uneven crystallization. Consequently, SALDI-MSI has become a highly promising analytical technique. This article systematically reviews the latest progress of nanomaterial-enhanced SALDI-MSI in spatial metabolomics. It first introduces various mass spectrometry imaging techniques used in spatial metabolomics, explains their working principles, and compares their advantages and disadvantages. Then, the fundamental mechanisms of SALDI are described to provide a theoretical basis for nanomaterial design, followed by a discussion of common sample preparation methods in SALDI-MSI. The review focuses on the design strategies and application cases of typical nanomaterials for SALDI-MSI, including metal/metal oxide nanoparticles, carbon-based materials, thin-film materials, and nanostructured silicon platforms. Finally, challenges and future directions in standardization, reproducibility, and quantification are discussed. This review aims to provide a reference for the rational design of high-performance SALDI substrates and to promote the development of spatial metabolomics.
    Keywords:  Mass spectrometry imaging; Metabolite analysis; Nanomaterials; SALDI-MSI; Spatial metabolomics
    DOI:  https://doi.org/10.1007/s00216-026-06597-w
  24. J Am Soc Mass Spectrom. 2026 Jun 05.
    Untargeted microLC-HRMS/MS for Measuring Endogenous Steroids in Mouse Plasma and Human Serum Samples Applied to Studying Polycystic Ovary Syndrome.
    Nathan Ghafari, Danko Brukner, Sherin A Nawaito, Danielle E Berbrier, Charlotte W Usselman, Nicolas Pilon, Lekha Sleno.
      Steroids play essential roles in regulating metabolism, response to stress, electrolyte balance, and reproductive function; however, their analysis in complex biological matrices remains challenging. Low endogenous concentrations, structural similarities, and poor ionization efficiencies can limit their detection, and conventional workflows frequently require large sample volumes and/or chemical derivatization, often restricting quantitative applications to targeted analyses. A workflow was developed for the untargeted analysis of endogenous steroids in serum or plasma samples using microflow liquid chromatography coupled to high-resolution tandem mass spectrometry. The Evosep One LC platform, applied widely for bottom-up proteomics, was coupled to a Sciex ZenoTOF 7600 quadrupole-time-of-flight system to enable the separation and detection of unconjugated and sulfated steroids in low-volume serum and plasma samples. The method was tested with a range of analytical standards, demonstrating efficient chromatographic separation and detection with high-accuracy MS/MS for structural confirmation. A total of 13 unconjugated steroids were confirmed and detected from female mouse plasma and/or human serum in positive mode, whereas three sulfated steroids were detected exclusively in human serum using negative mode. The sulfated steroids were confirmed using in vitro incubations of the parent steroids. Considerable interspecies differences were observed, consistent with the known literature on steroid metabolism. In a transgenic mouse model developed to mimic a metabolic subtype of polycystic ovary syndrome (PCOS), significant alterations in corticosteroids were detected. In human serum samples, dehydroepiandrosterone and androstenedione were significantly elevated in PCOS patients compared with healthy volunteers. The observed relative changes in both species showed similarities to the steroid perturbation patterns previously reported in PCOS.
    Keywords:  endogenous steroids; high-resolution tandem mass spectrometry; microflow liquid chromatography; plasma; polycystic ovary syndrome; serum
    DOI:  https://doi.org/10.1021/jasms.6c00096
  25. J Am Soc Mass Spectrom. 2026 Jun 03.
    Rapid On-Site Analysis of Psychotropic Drugs in Dried Blood Spots by Capillary-in-Capillary Electrospray Ionization (DBS-CC-ESI) Miniature Mass Spectrometry.
    Yiling Li, Jie Hong, Heyuan Jia, Xin Sui, Wei Xu, Yanbing Zhai, Ning Yuan.
      Therapeutic drug monitoring (TDM) of psychotropic agents is essential for optimizing therapeutic efficacy and minimizing adverse effects. However, conventional liquid chromatography-tandem mass spectrometry (LC-MS/MS) workflows are poorly suited for point-of-care applications due to labor-intensive sample preparation, prolonged turnaround times, and dependence on centralized analytical laboratories. Here, we present a rapid, on-site analytical platform that integrates dried blood spot (DBS) sampling with a modified capillary-in-capillary electrospray ionization (CC-ESI) source coupled to a miniature mass spectrometer (mini-MS). The sampling capillary was re-engineered as a disposable polypropylene microtube capable of accommodating a DBS punch and extraction solvent, thereby enabling fully integrated online extraction, ionization, and mass analysis within minutes. Critical parameters, including infrared drying duration and extraction solvent composition, were systematically optimized. The method demonstrated excellent linearity (R2 > 0.95) and precision for six widely prescribed psychotropic drugs: diazepam, flurazepam, clozapine, zolpidem, risperidone, and methaqualone. Analytical performance was comparable to that achieved using conventional solid-phase extraction, yet sample preparation time was reduced from several hours to mere minutes. Clinical utility was preliminarily demonstrated by the successful detection and confirmation of clozapine and aripiprazole in blood samples from patients receiving long-term pharmacotherapy. This DBS-CC-ESI-mini-MS platform represents a promising advance toward decentralized TDM of psychotropic drugs, offering minimal invasiveness, operational simplicity, and rapid, reliable quantitative capability.
    DOI:  https://doi.org/10.1021/jasms.6c00148
  26. BMC Bioinformatics. 2026 Jun 04.
    LipidCruncher: an open-source platform for processing, visualizing, and analyzing lipidomic data.
    Hamed Abdi, Yohannes A Ambaw, Zon Weng Lai, Ritchie Ly, Chandramohan Chitraju, Shubham Singh, Robert V Farese, Tobias C Walther.
       BACKGROUND: Advances in mass spectrometry (MS)-based lipidomics have led to a significant surge in data volume, underscoring a need for robust tools to efficiently evaluate and visualize these expansive datasets. While numerous software tools have been developed, current workflows are hindered by manual spreadsheet handling and insufficient data quality assessment prior to analysis. Here, we introduce LipidCruncher, an open-source, web-based platform designed to easily process, visualize, and analyze lipidomic data with high efficiency and rigor.
    RESULTS: LipidCruncher consolidates key steps of the lipidomics analysis workflow, including data standardization, normalization, and stringent quality controls. The platform also provides advanced visualization and analysis tools that are tailored to interrogate lipidomic data and enable detailed and holistic data exploration. To illustrate LipidCruncher's utility, we analyzed lipidomic data from adipose tissue of mice lacking the triacylglycerol synthesis enzymes DGAT1 and DGAT2.
    CONCLUSIONS: LipidCruncher fills a specific gap in the lipidomics analysis ecosystem by providing an integrated, quality-focused platform that accepts data from multiple sources and complements existing specialized tools. By bridging the critical divide between data generation and biological interpretation, LipidCruncher facilitates rigorous lipidomics analyses to accelerate the translation of complex lipid profiles into biological insights.
    Keywords:  Bioinformatics; Computational biology; Lipidomics; Lipids; Mass spectrometry; Open-source software; Phospholipids; Scientific software; Sphingolipids; Sterols
    DOI:  https://doi.org/10.1186/s12859-026-06483-3
  27. J AOAC Int. 2026 Jun 02. pii: qsag045. [Epub ahead of print]
    Simultaneous Determination of Four Per- and Polyfluoroalkyl Substances (PFAS) in DHA Products using LC-MS/MS for Quality Control and Risk Assessment.
    Jiayi Zhang, Yanping Cao, Xuee Xi, Chaoqiang Xiao, Li Zhu.
       BACKGROUND: Docosahexaenoic acid (DHA) is a critical dietary supplement for vulnerable populations (e.g., infants, pregnant women), but contamination by per- and polyfluoroalkyl substances (PFAS)-persistent "forever chemicals"-poses potential health risks. Currently, no standardized methods exist for PFAS detection in DHA products, hindering quality control and risk assessment.
    OBJECTIVE: To develop and validate a sensitive LC-MS/MS method for simultaneous determination of four PFAS (PFOA, PFODA, PFOS, and PFBS) in DHA matrices (algal oil and fish oil) and support product safety evaluation.
    METHODS: Samples were extracted with 50% methanol/acetonitrile (v/v) via ultrasonication (40 °C, 20 min), followed by centrifugation and filtration. Chromatographic separation was achieved on a Phenomenex Kinetex F5 column (100 × 3.0 mm, 2.6 μm) with gradient elution (mobile phase: 2 mmol/L ammonium formate aqueous solution-methanol) in 12 min. Detection was performed via negative electrospray ionization (ESI-) in multiple reaction monitoring (MRM) mode. Method validation included linearity, limits of detection (LODs)/quantitation (LOQs), accuracy, precision, matrix effects, and stability. Thirteen commercial DHA products (11 algal oil, 2 fish oil) were analyzed.
    RESULTS: Linearity (r ≥ 0.99) were achieved for PFAS; LODs/LOQs: 0.02/0.04 ng/mL. Recoveries at three spiking levels (0.1, 0.5, 1.0, 1.5 ng/mL) were ranged from 92.1%-108.4%, with RSDs of 2.8%-5.6%. Matrix effects were effectively corrected via matrix-matched calibration. Trace PFAS were detected in 3/13 samples, all below regulatory limits.
    CONCLUSIONS: The developed method is reliable for routine PFAS detection in DHA matrixes, providing practical technical support for quality control and risk assessment for DHA supplements for vulnerable populations.
    HIGHLIGHTS: Rapid (12 min), sensitive, and applicable to both algal oil and fish oil matrixes.
    Keywords:  DHA; LC-MS/MS; dietary supplement; food safety; per- and polyfluoroalkyl substances (PFAS); quality control
    DOI:  https://doi.org/10.1093/jaoacint/qsag045
  28. Anal Chem. 2026 May 30.
    MS-Net: Multi-Similarity-Based Network Annotation for Untargeted Metabolomics.
    Victor Pereira Francisco, Simon Duthen, Elise Crossay, Amélie Perez, Solweig Hennechart, Marion Alignan, Romain Valentin, Franck Milone-Delacourt, Guillaume Marti.
      Confident metabolite annotation remains a critical bottleneck in untargeted LC-MS metabolomics, with experimental spectral libraries covering only 5-20% of detected features. While in silico tools generate extensive candidate lists per feature, top-ranked predictions frequently fail to reflect true molecular identities, leading to high false annotation rates. We present multi-similarity Network-based annotation (MS-Net), an accessible workflow that integrates mass spectral similarity networks, molecular structure similarity (Tanimoto metrics), and taxonomic knowledge to prioritize annotations within vast candidate spaces. High-confidence annotations from authentic standards, spectral libraries, and taxonomically filtered candidates seed iterative propagation throughout mass spectral similarity networks. The workflow employs a composite Link Score combining structural, spectral, and computational evidence to rescue correct annotations from lower-ranked positions. Applied to Cannabis sativa extracts (2595 features to 1297 after filtering), MS-Net assigned 1275 compounds from an initial candidate space of over 118,000 structures. Notably, 53% of final annotations were rescued from ranks 2-50, demonstrating correction of initial in silico ranking. The workflow successfully reconstructed known cannabinoid biosynthetic pathways, validating biological coherence. MS-Net is freely available as a KNIME workflow with complete documentation at https://forge.inrae.fr/metatoul/equipe-agromix/ms-net, enabling reproducible, offline annotation suitable for systems biology integration.
    DOI:  https://doi.org/10.1021/acs.analchem.6c01026
  29. J Pharm Anal. 2026 May;16(5): 101472
    Extraction and determination of sartans: Recent advances and analytical perspectives.
    Peng-Li Wei, Yuan Zhang, Cheng Du, Xue-Song Feng, Xiao-Dan Liu.
      Sartans are essential antihypertensive drugs requiring reliable analytical methods for quality and efficacy monitoring. This review provides a comprehensive overview of recent analytical advances for sartans, focusing on pretreatment and detection methods. For sample preparation, conventional methods like protein precipitation, liquid-liquid extraction (LLE) and solid-phase extraction (SPE) have been optimized through the adoption of green solvents and automation. Emerging novel microextraction techniques including liquid phase microextraction and solid phase microextraction, in combination with advanced materials improve selectivity, especially for complex biological matrices. In the realm of detection, liquid chromatography-mass spectrometry (LC-MS) remains dominant, with high-resolution mass spectrometry (HRMS) (time-of-flight, orbitrap) enabling trace-level quantification and structural identification, outperforming traditional low-resolution mass spectrometry (LRMS). Emerging sensors offer rapid screening but lack MS-level multiplexing capability. The choice of methods should be based on sample complexity and analytical needs: biological samples benefit from microextraction-HRMS combinations, whereas pharmaceutical analysis may use simpler SPE-LC/MS workflows. Future directions should emphasize miniaturized, automated, and eco-friendly approaches to enhance throughput while reducing environmental impact. This review serves as a practical guide for selecting suitable strategies for the analysis of sartans across diverse analytical scenarios.
    Keywords:  Mass spectrometry; Microextraction; Sartans; Solid-phase extraction
    DOI:  https://doi.org/10.1016/j.jpha.2025.101472
  30. Forensic Toxicol. 2026 Jun 06.
    Metabolite patterns in human urine after oral administration of highly purified Δ8-THCV.
    Cristina Sempio, Jorge Campos-Palomino, Jelena Klawitter, Erica N Peters, Laura MacNair, Mehdi Haghdoost, Marcel Bonn-Miller, Amy Harrison, Shanna Babalonis, Marilyn A Huestis, Uwe Christians, Jost Klawitter.
       INTRODUCTION: The interest in therapeutic applications of tetrahydrocannabivarin (THCV) recently increased. For this reason, we validated an online extraction liquid chromatography- tandem mass spectrometry (LC-MS/MS) method to investigate the formation of urinary metabolites and understand potential cross-reactivity of THCV metabolites in cannabinoid immunoassays.
    METHOD: Urine samples were obtained after oral administration of Δ8-THCV to healthy participants. The protocol was approved by the Advarra Institutional Review Board (Pro00059879; approved December 20, 2021) and the trial was registered on clinicaltrials.gov (NCT05210634). Urine samples were collected pre-dose and pooled 0-8 hours post-dose. Urine samples were extracted using a simple one-step protein precipitation procedure and the extracts analyzed using online trapping LC-MS/MS in positive multiple reaction monitoring mode.
    RESULTS AND DISCUSSION: All compounds passed validation criteria in urine. In the clinical samples, 11-nor-9-carboxy-Δ8-THCV (Δ8-THCV-COOH) was the main metabolite detected before and after incubation with glucuronidases. Of the urine pooled 0-8 hours post-dose, 70 out of 80 were reported positive by a cannabinoid immunoassay targeting Δ9-THC-COOH, despite being negative for Δ9-THC-COOH and positive mainly for Δ8-THCV-COOH in the LC-MS/MS analysis.
    CONCLUSIONS: The major metabolites of Δ8-THCV in urine were Δ8-THCV-COOH, 11-hydroxy-Δ8-THCV and Δ9-THCV-COOH that were extensively glucuronidated and cross-react with immunoassay routinely used for toxicology testing resulting in false positive results for Δ9-THC exposure.
    Keywords:  Isomers; LC-MS/MS; Metabolites; THCV; Δ8-THC; Δ9-THC
    DOI:  https://doi.org/10.1007/s11419-026-00772-5
  31. Anal Chim Acta. 2026 Sep 01. pii: S0003-2670(26)00592-1. [Epub ahead of print]1413 345642
    Comprehensive investigation of matrix effect evaluation approaches for reliable quantification in bioanalysis using UHPLC-MS/MS.
    Hana Kočová Vlčková, Kateřina Plachká, František Švec, Lucie Nováková.
       BACKGROUND: Matrix effect (ME) evaluation is an indispensable part of the method development and validation when using ultra-high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS). The rotational and translational matrix effects are often observed. The rotational matrix effect depends on the analyte concentration and affects the slope of the calibration function, while the translational matrix effect is independent of the analyte concentration and affects the intercept of the calibration function. Two matrix effect evaluation strategies, the post-extraction addition and the comparison of calibration curve slopes, are the most widely used for the quantitative ME evaluation. The post-extraction addition approach recommended by the European Medicines Agency (EMA) guideline is considered the reference approach. However, the extent to which these approaches provide comparable results has not been systematically assessed.
    RESULTS: We evaluated the suitability of the calibration curve slope approach for quantifying ME. Two ME evaluation strategies were systematically compared using ESI-UHPLC-MS/MS in both negative and positive ionization modes for the analysis of 26 compounds in serum. Various calibration models, including 1/X0, 1/X, and 1/X2 weighting or logarithmic transformation, were assessed. None of the tested models provided overestimated results compared to the post-extraction addition approach. However, several models exhibited underestimated results. Thus, we developed a new approach for calculation of ME taking into account also the translational ME expressed by the intercept of the calibration curve. The accuracy of the new approach was subsequently determined using three different matrices and two different instrumental platforms.
    SIGNIFICANCE: It is not advisable to rely solely on the calibration curve slope approach for accurate estimation of ME unless translational ME derived from calibration curve intercept are also involved in calculation. Therefore, a novel intercept-based equation was proposed for the calculation of translational matrix effects. The total matrix effect, obtained as the sum of the slope- and intercept-derived contributions, closely corresponds to matrix effects determined by the post-extraction addition approach.
    Keywords:  Calibration curve slope; Calibration model; Mass spectrometry; Matrix effect; Post-extraction addition
    DOI:  https://doi.org/10.1016/j.aca.2026.345642
  32. Se Pu. 2026 Jun;44(6): 694-704
    [Determination of 40 carbonyl compounds in ambient air by high performance liquid chromatography-triple quadrupole mass spectrometry].
    Guang-Hui Li, Shuo Deng, Qin-Qin Li, Chun-Lin Zhang, Yun-Feng Liu, Bin Jiang, Qian Yao, Hao Wang, Bo-Guang Wang.
      Carbonyl compounds （CCs） are a pivotal class of oxygenated volatile organic compounds in ambient air， which are mainly derived from natural emissions， primary emissions from anthropogenic sources， and secondary formation due to atmospheric oxidation. Various classes of CCs have different impacts on human health， and play critical roles in atmospheric photochemical reactions， ozone production， and the formation of secondary organic aerosols. At present， the number of CCs in ambient air determined by traditional methods is limited， especially for high molecular weight monocarbonyl compounds （HMW-MCs） and dicarbonyl compounds （DCs）. If more CCs can be accurately determined， it will be beneficial for the study of atmospheric oxidation mechanisms and the formulation of pollution control strategies.In this study， an analytical method was developed that enables simultaneous determination of the 40 CCs in ambient air with a single injection， utilizing high-performance liquid chromatography-triple quadrupole mass spectrometry. First， the 16 CCs-2，4-dinitrophenylhydrazine （DNPH）-derivatized single standards were prepared using purified DNPH crystals in the laboratory. Second， the remaining 24 commercial CCs-DNPH-derivatized hybrid standards were purchased. Finally， all the above standards were mixed in a certain proportion to prepare the 40 CCs-DNPH-derivatized hybrid standards for later use. The sample collection procedures （sampling flow rate and sampling duration）， the pretreatment methods （elution volume and constant volume）， the chromatographic analysis conditions （chromatographic column， the concentration of ammonium acetate， etc.） and the mass spectrometry analysis conditions （ion source parameters， fragmentation voltage， collision energy， etc.） were optimized. Ambient air samples were collected using DNPH cartridges （at a flow rate of 1 L/min， for 4 h）， eluted with 4 mL of acetonitrile and diluted to a final volume of 5 mL （the acetonitrile naturally flowed through the DNPH cartridges in the opposite direction to the sampling direction） in a vacuum drying chamber， and then filtered through a 0.22 μm organic filter membrane and transferred to 1.5 mL brown sample bottles prior to instrumental analysis. Chromatographic separation was performed using a Sepax BR-C18 column （250 mm×4.6 mm， 5 μm） with mobile phases consisting of 1.0 mmol/L ammonium aqueous solution and acetonitrile under gradient elution conditions. The analysis was performed at a column temperature of 50 ℃ with an injection volume of 5 μL. The target analytes were identified using negative electrospray ionization （ESI-） and multiple reaction monitoring （MRM） modes and quantified using the external standard method. The results showed that the 40 CCs exhibited good linearities within the mass concentration range of 2.5-200 μg/L， with the determination coefficients （R2） exceeding 0.997 8. The method detection limits and method quantification limits were established within the ranges of 0.001-0.03 μg/m3 and 0.005-0.12 μg/m3， respectively. The blank spiked recoveries of the target analytes at low， middle， and high concentration levels （0.05， 0.1， and 0.2 μg） ranged from 75.2% to 119.0%， while the relative standard deviations （RSDs， n=7） ranged from 0.4% to 4.2%. This analytical method was applied to the monitoring of ambient samples in the Pearl River Delta region. Except for 2-furaldehyde and isophorone， 38 CCs were effectively detected. Among these， formaldehyde， acetaldehyde and nonanal consistently showed higher concentrations across all sampling sites. Overall， the concentrations of low molecular weight monocarbonyl compounds （LMW-MCs） were moderately higher than those of HMW-MCs， and substantially higher than those of DCs. Compared with conventional methods， this method effectively overcame the limitations in existing approaches regarding the limited variety and detection difficulties of DCs and HMW-MCs. Additionally， it also improved the chromatographic resolution of target analytes which have similar retention times and the same ion pairs. Overall， this method was simple and rapid， offering excellent sensitivity， precision， and chromatographic resolution. It was suitable for the determination of the abovementioned 40 CCs in ambient air．.
    Keywords:  ambient air; carbonyl compounds （CCs）; high performance liquid chromatography-triple quadrupole mass spectrometry （HPLC-MS/MS）
    DOI:  https://doi.org/10.3724/SP.J.1123.2025.04028
  33. J Am Soc Mass Spectrom. 2026 Jun 05.
    Pseudoenhanced Peak Efficiency in Liquid Chromatography-High Resolution Mass Spectrometry Using Multiple Second Derivatives.
    Guillaume Laurent Erny.
      A mathematical approach is introduced to achieve pseudoenhanced peak efficiency in liquid chromatography-high resolution mass spectrometry (LC-HRMS1), utilizing second-derivative transformations with respect to time and Gaussian smoothing cycles. The pipeline involved interpolating all MS scans, recorded as profile scans, onto a common m/z axis, allowing for second-derivative transformations for each m/z increment with respect to time across the entire data set. Validation using a public study (comprising 1100 compounds analyzed on a Thermo Q Exactive) demonstrates substantial improvements in feature detection and resolution, with qualitative and quantitative benefits. The transformation enables increased peak efficiency by up to 2 orders of magnitude in multicycle implementations without requiring physical hardware enhancements. The approach provides enhanced separation of complex mixtures, reduced background contributions, and increased reliability in untargeted metabolomics and related analyses.
    DOI:  https://doi.org/10.1021/jasms.5c00315
  34. J Chromatogr B Analyt Technol Biomed Life Sci. 2026 May 28. pii: S1570-0232(26)00235-7. [Epub ahead of print]1281 125146
    Determination and stereoselective pharmacokinetics of fluralaner enantiomers in broiler chickens by liquid chromatography-tandem mass spectrometry.
    Tong Zhou, Yahao Ding, Xun Liu, Zhengwen Wang, Rong Liu, Limin He.
      Fluralaner (FLL) is a newly developed broad-spectrum isoxazoline acaricide. It is a chiral compound, with only the S-enantiomer exhibiting high activity. In this study, we developed a chiral liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to quantify FLL enantiomers in broiler chicken plasma, and subsequently applied it to study stereoselective pharmacokinetics. Two cyclic polypeptides, one cyclic saccharide and three cellulose Derivative chromatographic chiral columns were evaluated. The cellulose tris (4-methylbenzoate) superficially porous particle column (150 mm × 2.1 mm i.d., 3.0 μm) achieved optimal separation of the two enantiomers within six minutes. Molecular docking analysis suggests that π-π stacked interactions are a primary mechanism for the separation of enantiomers, as evidenced by their critical role in molecular recognition and stabilization. The isotopic internal standard dilution method was used for quantification and eliminating matrix effects, and the developed method exhibited good linearity over the range of 5-200 ng mL-1 (r2 ≥ 0.99) for both S-FLL and R-FLL. The accuracy for two enantiomers at quality control concentration levels of 5 (lower limit of quantification), 10, 75 and 180 ng mL-1 were 96.3% to 104.3% in broiler chicken plasma, with coefficient of variation below 4.7%. Pharmacokinetic analysis indicated that the inactive R-enantiomer of FLL exhibited a greater maximum concentration (Cmax) and a larger area under the curve (AUC) compared to the S-enantiomer, suggesting a higher exposure to the drug. Conversely, the S-enantiomer showed a more rapid clearance rate, indicating a faster stereoselective elimination from the body. Dosing strategies must account for enantiomer-specific behavior to maximize efficacy.
    Keywords:  Broiler chicken; Enantiomers; Fluralaner; Liquid chromatography-tandem mass spectrometry; Stereoselective pharmacokinetics
    DOI:  https://doi.org/10.1016/j.jchromb.2026.125146
  35. Anal Bioanal Chem. 2026 Jun 02.
    Isotope dilution LC-MS/MS for the quantification of ergot alkaloids: a comparative study.
    Sven-Oliver Herter, Susanne Krentscher, Kevin Sassin, Christian Kornrumpf, Sarah Kulas, Hajo Haase, Matthias Koch.
      Ergot alkaloids (EAs) are toxic secondary metabolites formed by various fungi, most notably Claviceps purpurea, which infects cereal crops such as rye, wheat, and barley. Due to their toxicity, the European Commission established maximum levels for 12 priority EAs in cereals and related products in 2022. Routine monitoring, typically employing high-performance liquid chromatography coupled to tandem mass spectrometry, is challenged by the unavailability of isotope-labeled internal standards. To address this, we previously synthesized internal standards (ISTDs) for 12 priority EAs and herein we evaluate their performance through an interlaboratory comparison against the standard addition approach prescribed in EN 17425. The ISTDs significantly improved method precision and trueness, with results in good agreement across both laboratories. Furthermore, we developed a reference material for EAs in rye flour, in accordance with ISO 33405 guidelines, using stable isotope dilution mass spectrometry as primary method. This internal RM contributes to safer foodstuffs by supporting reliable method development and validation for EAs.
    Keywords:  Cereals; Ergot alkaloids ; HPLC-MS/MS; Internal standard; Reference material
    DOI:  https://doi.org/10.1007/s00216-026-06581-4
  36. Talanta. 2026 Jun 01. pii: S0039-9140(26)00726-5. [Epub ahead of print]310 130070
    Analytical validation of a dried blood microsampling method to measure androstenedione, 17α‑hydroxyprogesterone, and 11‑ketotestosterone for congenital adrenal hyperplasia monitoring.
    Hanna De Baets, Tim Reyns, Monica Mazzarino, Tom Fiers, Peter Van Eenoo, Christophe P Stove.
      Measurement of androstenedione (4-AD) and 17α-hydroxyprogesterone (17-OHP) in blood is crucial for diagnosing and monitoring endocrine disorders such as congenital adrenal hyperplasia (CAH), which results from enzymatic defects in the steroidogenesis pathway. CAH patients require lifelong hormone replacement therapy to manage adrenal insufficiency and control androgen excess. Microsampling offers a less invasive alternative to frequent venous blood sampling, particularly in paediatric CAH patients, and enables at-home monitoring. Including 11-ketotestosterone (11-KT), an emerging biomarker in CAH, further enhances the clinical relevance of this approach. Liquid chromatography-tandem mass spectrometry-based methods were established and fully validated for the determination of 4-AD, 17-OHP and 11-KT in plasma, blood and 20 μL dried blood microsamples collected by volumetric absorptive microsampling (VAMS). For VAMS samples, we paid particular attention to robustness regarding storage and hematocrit to support future home sampling applications. The method's applicability was evaluated by assessing the agreement with plasma as the reference matrix for steroid hormone determination. A robust extraction procedure was developed, ensuring consistent recoveries across storage conditions and hematocrits (0.20 - 0.60 L/L). The method was successfully validated for 4-AD, 17-OHP and 11-KT in VAMS, blood and plasma samples, achieving lower limits of quantification of 30, 144 and 81 pg/mL in VAMS samples, respectively. Accuracy and precision were within 6.6% and 14.0% for all matrices. VAMS samples remained stable for up to one week at room temperature and after postal sending. A proof-of-concept study showed that plasma concentrations can reliably be derived from VAMS concentrations, when taking into account the hematocrit.
    Keywords:  11-Ketotestosterone; 17α-hydroxyprogesterone; Androstenedione; Congenital adrenal hyperplasia (CAH); Liquid-chromatography-tandem mass spectrometry (LC-MS/MS); Volumetric absorptive microsampling (VAMS)
    DOI:  https://doi.org/10.1016/j.talanta.2026.130070
  37. Clin Chim Acta. 2026 Jun 01. pii: S0009-8981(26)00310-4. [Epub ahead of print] 121128
    Mass spectrometry in laboratory medicine: advances in automation, multiplex biomarker quantification, and diagnostics.
    Farida Khamidova, Ugilzhan Tatykayeva, Gulsara Reymnazarova, Shakhnoza Davronova, Ikrom Tilyabov, Shakhboz Khasanov.
      Mass spectrometry (MS) has evolved from a specialized research tool into an increasingly indispensable platform in laboratory medicine. Its clinical value is driven by molecular specificity, multiplex quantification, and the ability to measure small molecules, peptides, proteins, drugs, metabolites, and microbial spectral fingerprints in workflows that are becoming more automated and standardized. The field is nevertheless heterogeneous: liquid chromatography-tandem mass spectrometry (LC-MS/MS), matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), gas chromatography-mass spectrometry (GC-MS), and emerging high-resolution or miniature instruments address different clinical questions and require different validation strategies. The review focuses on the realistic transition of MS from specialist reference laboratories to routine clinical practice. It summarizes fundamental principles of MS measurement, current clinical platforms, microbial identification by MALDI-TOF MS, automated monoclonal protein analysis, LC-MS/MS steroid and therapeutic drug monitoring, GC-MS applications, MassARRAY genotyping, pre-analytical vulnerabilities, and barriers to implementation. Fully automated MALDI-TOF MS platforms (e.g., EXENT) now achieve 92.6-95.7% concordance with conventional electrophoresis for monoclonal immunoglobulin detection while showing superior sensitivity for low-concentration M-proteins. Multiplex LC-MS/MS panels enable simultaneous quantification of 23 plasma steroids and 15 protein-bound uremic toxins with excellent linearity and precision, whereas MassARRAY-based genotyping has achieved 99.75% detection success in newborn screening for primary carnitine deficiency. Critical remaining limitations include incomplete inter-laboratory harmonization, high capital and maintenance costs, the need for trained personnel, matrix effects, pre-analytical instability, limited evidence for some biomarker panels, and uncertain regulatory pathways for laboratory-developed tests. The strongest near-term applicability is expected in high-volume, well-validated use cases - newborn screening, therapeutic drug monitoring, steroid profiling, toxicology, microbial identification, monoclonal protein testing, and selected multiplex biomarker panels - rather than unrestricted replacement of immunoassays. The future relevance of clinical MS is likely to remain strong, provided that automation is coupled with rigorous analytical validation, external quality assessment, and clear demonstration of clinical utility.
    Keywords:  Automation; Clinical chemistry; Gas chromatography-mass spectrometry; Liquid chromatography-tandem mass spectrometry; Mass spectrometry; Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry; Metabolomics; Newborn screening; Pre-analytical factors; Steroid profiling; Therapeutic drug monitoring
    DOI:  https://doi.org/10.1016/j.cca.2026.121128
  38. Se Pu. 2026 Jun;44(6): 658-666
    [Determination of seven tire antioxidants and their quinone oxidation products in fine particulate matter by high performance liquid chromatography-tandem mass spectrometry].
    Feng Liu, Bin-Bin Tang, Li-Yuan Wu, Li-Xin Song, Min Zhang, Min He.
      p-Phenylenediamine compounds （PPDs） are widely used as anti-aging agents and antioxidants in rubber industry. However， environmental concerns have arisen regarding the toxicity of their quinone derivatives （PPD-Qs）. Fine particulate matter （PM2.5） serves as a crucial vector enabling PPDs and PPD-Qs to enter the human body via respiratory exposure pathway. Therefore， accurate monitoring of PPDs and PPD-Qs in PM2.5 is essential. In this research， a high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） approach was established to quantify seven PPDs and seven PPD-Qs in PM2.5. Samples were collected on quartz fiber filters with a diameter of 90 mm. The filter was cut into strips and subsequently spiked with 2 ng of 6PPD-d5 and 6PPD-Q-d5 internal standards. The target compounds were extracted with 10 mL of acetonitrile containing 1% （volume fraction） ammonia solution and 20 μmol/L glutathione （GSH）， and purified via a modified QuEChERS pretreatment method. Specifically， after salting out with 0.5 g of NaCl and 1.0 g of MgSO4， the supernatant was subjected to dispersive solid-phase extraction for cleanup. In this process， 0.5 g of MgSO4， 100 mg of octadecylsilane （C18）， and 100 mg of N-propylethylenediamine （PSA） were employed as sorbents. Subsequently， 5 mL of the cleaned-up supernatant was evaporated to near dryness and then redissolved in 0.2 mL of a methanol-water mixture （1∶1， volume ratio） for instrumental determination. The compounds were separated on a Waters ACQUITY UPLC HSS T3 column（100 mm×2.1 mm，1.8 μm） with mobile phases consisting of a 5 mmol/L ammonium formate aqueous solution containing 0.1% formic acid and methanol. Identification and quantification of the compounds were carried out under positive electrospray ionization in multiple reaction monitoring mode. The results indicated that all analytes exhibited good linear relationships within the range of 0.05-20.0 ng/mL， with correlation coefficients （r） exceeding 0.999. The method detection limits （MDLs） and method quantification limits （MQLs） of the compounds were within the ranges of 0.003-0.07 pg/m3 and 0.01-0.2 pg/m3， respectively. At three spiked levels of low， medium and high， the recoveries of the compounds were in the range of 66.3% to 119.0% ， and the relative standard deviations （RSDs） ranged from 1.5% to 13.2% （n=6）. Ultimately， the developed method was employed for the analysis of PPDs and PPD-Qs in PM2.5 samples collected from Baotou during January and February 2025. The results indicated that seven PPDs and five PPD-Qs were detected， with mass concentrations ranging from 2.26 to 251.2 pg/m3 and 2.36 to 105.4 pg/m3， respectively. The proposed method is characterized by its simplicity， environmental friendliness and accuracy， making it suitable for the rapid quantitative analysis of PPDs and PPD-Qs in PM2.5.
    Keywords:  fine particulate matter （PM2.5）; high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）; p-phenylenediamine compounds （PPDs）; p-phenylenediamine quinones （PPD-Qs）
    DOI:  https://doi.org/10.3724/SP.J.1123.2025.09023
  39. J Chromatogr A. 2026 Jun 01. pii: S0021-9673(26)00482-6. [Epub ahead of print]1783 467153
    Streamlined LC-HRMS-based determination of sterols and triterpenic alcohols in edible oils for authentication purposes.
    Irene Caño-Carrillo, Beatrice Schiavone, Andrés J Rascón, Bienvenida Gilbert-López, Juan F García-Reyes.
      Sterol analysis is a key parameter for assessing the authenticity and quality of olive oil, as defined by official methods. Nevertheless, these protocols are labor-intensive and require multiple preparation steps, including sample fractionation and derivatization. In the present work, a simplified analytical methodology is proposed for the determination of free sterols and triterpenic alcohols, eliminating these time-consuming procedures. The method is based on the direct analysis of saponified extracts, prepared according to the official protocol, followed by a single dilution step and analysis by liquid chromatography coupled to high-resolution mass spectrometry with electrospray ionization (LC-ESI-HRMS). To enhance the ionization efficiency of free sterols, which exhibit low response under conventional ESI conditions due to their non-polar nature, ammonium formate was added to the mobile phase. The analytical performance of the method was evaluated in terms of linearity, reproducibility, and limits of quantification to support its suitability for comparative fingerprinting analysis. Based on the obtained sterol profiles, several compounds were identified as potential markers for differentiating edible oils, including extra virgin olive oil, pomace olive oil, rapeseed oil, avocado oil, almond oil, and sunflower oil. The application of principal component analysis (PCA) to these data further enabled the distinction of extra virgin olive oil from the remaining vegetable oils, demonstrating the discriminatory potential of the proposed approach for oil characterization and classification.
    Keywords:  Authentication; Edible oils; LC-MS; Mass spectrometry; Olive oil; Sterols
    DOI:  https://doi.org/10.1016/j.chroma.2026.467153
  40. J AOAC Int. 2026 Jun 02. pii: qsag047. [Epub ahead of print]
    An Integrated QuEChERS LC-MS/MS Method for Screening, Confirmation, and Quantification of Nitroimidazole Residues in Food.
    Hoi-Yan Fiona Shiu, Kong-Chi Lau, Ho-Pan Michael Yau.
       BACKGROUND: Nitroimidazoles are prohibited veterinary drugs, for which sensitive and reliable analytical methods are required for regulatory residue control in food, particularly across diverse and complex matrices.
    OBJECTIVE: This study aimed to develop an integrated QuEChERS-LC-MS/MS method for screening, confirmatory identification, and quantitative determination of nitroimidazole residues within a single harmonized analytical workflow.
    METHODS: Samples were prepared using a unified QuEChERS procedure followed by dispersive solid-phase clean-up and LC-MS/MS analysis with isotope-labelled internal standards. Screening was conducted using a predefined screening target concentration (STC) as a validation reference level. Samples meeting relative retention time requirements and exhibiting responses exceeding a conservative screening cut-off were classified as suspected positives and subjected to confirmatory evaluation based on ion ratio criteria, followed by quantitative determination within the same analytical run. The method was validated for muscle, offal, fat, milk, egg, and aquatic products. Decision limits (CCα) and detection capabilities (CCβ) were established in accordance with regulatory guidelines.
    RESULTS: Excellent linearity was obtained (r2 ≥ 0.99) over the range of 0-2.5 µg/L. Mean recoveries ranged from 84 to 116%, with RSDs 0.1-8.1%. Limits of quantification were 0.2-0.4 µg/kg across all matrices, and matrix effects were adequately controlled (91-110%).
    CONCLUSION: The validated method provides a robust and harmonized analytical workflow suitable for screening, confirmation, and quantification of nitroimidazole residues across a wide range of food matrices, supporting regulatory residue control.
    HIGHLIGHTS: A single harmonized QuEChERS-LC-MS/MS workflow was developed for the screening, confirmatory identification, and quantitative determination of four nitroimidazoles and their metabolites in animal and aquatic foods. The method applies an STC-based decision strategy with confirmatory identification criteria and was validated across multiple matrices, achieving low LOQs. Performance was evaluated in accordance with Commission Implementing Regulation (EU) 2021/808 and verified through international proficiency testing.
    DOI:  https://doi.org/10.1093/jaoacint/qsag047
  41. bioRxiv. 2026 May 29. pii: 2026.05.27.728049. [Epub ahead of print]
    Translational Quantitative Proteomic Assay for Bacteriophages: A New Frontier in Phage Pharmaceutical Development.
    Thomas D Nguyen, Connor E Gould, Jacob T Sanborn, Joshua Tutin, Yan Pan, Haoran Gao, Donna Ruszaj, Devin Agevine, Johnathan Bussa, Daniel Atakora, Liang Chen, Dwayne R Roach, Troy D Wood, Nicholas M Smith.
      Accurate quantitation of therapeutic bacteriophages ( phages ) remains a challenge for clinical development. Plaque-based enumeration is the current standard but is laborious, host-dependent, and variable, particularly when distinguishing individual phages in cocktails. Targeted mass spectrometry of virion structural proteins offers an orthogonal, structure-based approach amenable to reproducible and scalable phage quantitation. Here, we describe a targeted proteomic liquid chromatography-tandem mass spectrometry ( LC-MS/MS ) assay for host-independent quantitation of the Pseudomonas aeruginosa podovirus LUZ19. Proteomic characterization was performed on an LTQ Orbitrap XL to assess sequence coverage and select surrogate peptide candidates based on specificity and sensitivity. High-resolution peptide mapping identified multiple structural proteins of LUZ19 and provided 55% sequence coverage for the major head protein (YP_001671977.1). Fifteen peptides were detected and evaluated, from which the tryptic peptide EVAELDGQELAR was selected based on abundance, stability, and chromatographic performance. Quantitative analysis was conducted on a QTRAP 7500+ using optimized multiple reaction monitoring transitions for targeted peptide detection. Back-calculated concentrations met accuracy criteria across a validated range of 0.008 to 80 pg/mL, with bias spanning -8.2 to 8.2%, intra-day precision ranging from 0.5 to 9.8%, and inter-day precision ranging from 6.3 to 9.7%. Peptide concentrations from digested lysate samples were related to phage concentrations determined by double layer agar assay, yielding an estimated three copies of the major head protein per virion.
    Importance: Bacteriophages are the most abundant biological entities on the planet and represent a promising therapeutic class for combating drug-resistant bacterial infections. Realizing the clinical potential of bacteriophage therapy requires analytical methods capable of meeting the standards of modern drug development. Targeted mass spectrometry offers unmatched specificity and resolution for precise quantitation of individual bacteriophages within complex biological samples, a capability that conventional enumeration methods cannot match. Only one prior study has applied mass spectrometry to bacteriophage quantitation, using a well-characterized model bacteriophage at a single concentration without calibration or a validated analytical range. Using Pseudomonas aeruginosa podovirus LUZ19, we present the first targeted mass spectrometry-based bacteriophage quantitation assay developed and validated following FDA bioanalytical guidance. This work establishes a rigorous analytical foundation that moves bacteriophage therapy closer to the standards required for informed dose selection, candidate evaluation, and clinical development.
    DOI:  https://doi.org/10.64898/2026.05.27.728049
  42. Anal Chim Acta. 2026 Aug 22. pii: S0003-2670(26)00597-0. [Epub ahead of print]1412 345647
    Multi-residue analytical method of 215 pesticides in peanut by GC-Q-Orbitrap MS/MS.
    Xiaofan Qi, Sufang Fan, Lijun Han, Zhijuan Meng, Xiaoying Wan, Wenbo Zeng, Canping Pan.
      For the analysis of pesticides in the complex, high-fat matrix of peanuts, this study developed a high-throughput screening and quantitative method for 215 pesticide residues using gas chromatography-quadrupole Orbitrap high-resolution mass spectrometry (GC-Q-Orbitrap HRMS). The sample preparation workflow was systematically optimized. Peanut samples were extracted with acetonitrile containing 1% acetic acid, followed by salting-out with an acetate buffer salt mixture and purification through a multi-stage filtration column (m-PFC) packed with a novel LPAS adsorbent material. Under the optimized conditions, the method was validated at three spiking levels, delivering average recoveries for the 215 pesticides in the range of 70.7%-118.8%, with relative standard deviations (RSDs) between 1.1% and 9.2%. The distribution and correlation between chemical structures and retention behavior were analyzed to characterize the chromatographic separation capability and patterns for the large number of compounds. The established method is suitable for routine multi-residue monitoring of pesticides in peanuts, and the systematic optimization strategy also provides a reference for analyzing other complex matrices.
    Keywords:  Gas chromatography-quadrupole Orbitrap; High-resolution mass spectrometry; Method optimization; Peanuts; Residue analysis
    DOI:  https://doi.org/10.1016/j.aca.2026.345647
  43. Anal Chem. 2026 Jun 03.
    A Polysorbate Structural Atlas Curated from Drift Tube Ion Mobility-Mass Spectrometry Measurements.
    Kyle E Lira, Alexander D Goodness, Jody C May, John A McLean.
      Polysorbates (PSs) are mixtures of synthetic surfactants with widespread use in different application areas. PSs are particularly important in pharmaceutical and biotherapeutic formulations owing to their ability to minimize aggregation and surface adsorption. However, PSs are known to undergo degradation and autoxidation which can alter their efficacy. While studies have been conducted to better understand the chemical composition of PSs, comprehensive chemical characterization is challenging due to the heterogeneity of commercial PSs which contain numerous molecules representing both active surfactants and byproducts of synthesis. These complex mixtures result in extensive isomer and isobar species confounding characterization. Here, we utilize structurally selective drift tube ion mobility-mass spectrometry (DTIMS-MS) to compile a collision cross section (CCS) structural atlas for commonly found species in both polysorbate 20 and 80 (PS-20 and PS-80), two of the most commonly used PSs. This comprehensive IM-MS survey discovered a total of 536 molecules with discrete chemical formulas (350 in PS-20 and 186 species in PS-80), with each CCS measurement exhibiting high analytical reproducibility (<0.4% RSD, n ≥ 4 replicates). The primary chemical species found from electrospray spectra of US Pharmacopeia standards were singly charged monoesters and nonesterified species, with larger PS molecules favoring higher charge states. This first-of-a-kind, highly curated CCS database for PSs resulted in 41 empirically defined mobility-mass correlations (PS structure vs mass) that predict the location of individual PS oligomer species from IM-MS data for improved characterization.
    DOI:  https://doi.org/10.1021/acs.analchem.6c02138
  44. Anal Chim Acta. 2026 Aug 15. pii: S0003-2670(26)00587-8. [Epub ahead of print]1411 345637
    An LC-MS-guided AI enabled serum molecule-interpretable SERS platform for exploratory metabolomic analysis in Alzheimer's disease.
    Yanling Wang, Chi Zhang, Tong Liu, Qingsong Li, Xue Guan, Yutian Hu, Bo Cao, Xiaohong Wu, Qin Zhou, Feiyun Cui.
      Label-free surface-enhanced Raman spectroscopy (SERS) offers a promising avenue for rapid metabolic phenotyping in complex biofluids, yet its translational potential is hindered by the challenge of deconvoluting overlapping spectral contributions and identifying specific metabolite signatures. Herein, we report a liquid chromatography-mass spectrometry (LC-MS)-guided AI enabled serum molecule-interpretable SERS Platform, termed AMI-SERS, which integrates SERS, untargeted metabolomics and machine learning (ML) for Alzheimer's disease (AD) patient serum exploratory metabolic profiling. ML has achieved excellent classification performance with an accuracy of 96.67% under leave-one-out cross-validation. A novel multi-source matching algorithm was devised to trace dominant spectral features directly to specific metabolite changes, uncovering hypoxanthine as a key pre-analytical confounder and nominating adenine as a potential AD biomarker. However, due to the limited sample size, these results are only applicable to exploratory analysis. In conclusion, the AMI-SERS platform establishes a molecular-resolvable, LC-MS-interpretable AI methodological framework for exploratory serum metabolomics and its clinical applicability requires large-scale independent validation.
    Keywords:  Alzheimer's disease (AD); Machine learning (ML); Metabolism analysis; Surface-enhanced Raman spectroscopy (SERS)
    DOI:  https://doi.org/10.1016/j.aca.2026.345637
  45. Anal Chim Acta. 2026 Aug 15. pii: S0003-2670(26)00593-3. [Epub ahead of print]1411 345643
    Determination of short-chain chlorinated paraffins in marine sediment by automated online solid phase extraction coupled to liquid chromatography-high-resolution mass spectrometry.
    Feiyao Lu, Dan Fu, Xiuping He, Xueting Zhang, Haoshun Zhang, Tongzhu Han, Junhui Chen.
       BACKGROUND: Short-chain chlorinated paraffins (SCCPs) are emerging persistent organic pollutants that accumulate in marine sediments, threatening benthic organisms. Existing analytical workflows require laborious purification of crude sediment extracts (i.e., unpurified) to remove matrix interferences, with column chromatography remaining time-consuming and labor-intensive. This study develops an automated online solid-phase extraction (SPE)-liquid chromatography-high-resolution mass spectrometry (LC-HRMS) method for SCCP determination in crude sediment extracts without additional purification.
    RESULTS: Following extraction and concentration, crude sediment extracts were reconstituted in acetonitrile and analyzed by online SPE-LC-HRMS without additional purification. Satisfactory recoveries (71.9%-87.4%), sensitivity (LOD = 20.0 pg of ∑SCCPs on column), and repeatability (RSD < 15.0%) were achieved, with good concentration linearity (R2 > 0.990) and chlorine content linearity (R2 > 0.940). This approach greatly simplifies sample pretreatment while obtaining quantification results comparable to offline SPE purification. SCCPs were widely detected in surface sediments from a typical mariculture bay in northern China.
    SIGNIFICANCE: This method enables the determination of SCCPs in crude sediment extracts without additional purification, eliminating time-consuming column chromatography and substantially reducing the sample preparation time. The proposed method provides a useful tool for routine SCCPs determination in marine sediments, and promotes SCCPs monitoring and risk management in marine sedimentary environment.
    Keywords:  Marine sediments; Nearshore bay; Online solid phase extraction; Quadrupole time-of-flight mass spectrometry; Short-chain chlorinated paraffins
    DOI:  https://doi.org/10.1016/j.aca.2026.345643
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