Journal of Chromatography B最新文献

{"title":"UPLC-MS/MS-based targeted analysis of human serum revealed that aberrant arachidonic acid metabolism may contribute to the pathogenesis of type 2 diabetes mellitus","authors":"Peng Jin ,&nbsp;Kun Wang ,&nbsp;Xiao-wan Hu ,&nbsp;Yi-fan Yang ,&nbsp;Xian-jie Huang ,&nbsp;Yan Du ,&nbsp;Dao-quan Tang","doi":"10.1016/j.jchromb.2025.124871","DOIUrl":"10.1016/j.jchromb.2025.124871","url":null,"abstract":"<div><div>The aberrant arachidonic acid (ARA) metabolism may contribute to the pathogenesis of type 2 diabetes mellitus (T2DM), and some metabolites from ARA may have benefits for the differential diagnosis of T2DM. Thus, the aim of this study was to develop an ultra-high performance liquid phase coupled with mass spectrometry (UPLC-MS/MS) for determination of ARA and its 11 metabolites in the serum of patients with T2DM and explore the relation between ARA metabolites and T2DM pathogenesis. A cohort of 66 healthy individuals and 141 patients with T2DM enrolled from Suining People's Hospital Affiliated to Xuzhou Medical University was studied. The UPLC-MS/MS technique was developed and applied to obtain the serum ARA and its 11 metabolite profiles. Multivariate statistical analysis referring to metabolomics were applied for the metabolites data analysis and the differential metabolites screening. The results showed that a total number of 6 differential metabolites were presented between T2DM patients and healthy control subjects. Among these differential metabolites, (±)14(15)-epoxyeicosatrienoic acid (EET) presented the 1.64-fold elevation in T2DM patients versus healthy control subjects, significant correlation with biochemical index [fasting blood glucose (FBG) and glycated hemoglobin (HbA1c)] (<em>P</em> &lt; 0.01), and Receiver Operating Characteristic (ROC) area under the curve (AUC) of 0.6063 with the sensitivity of 26.95% and specificity of 93.94% (95% confidence interval, 0.5280–0.6846) for the diagnosis of T2DM. This study advances previous findings by establishing eicosatetraenoic acids flux imbalance as a hallmark of early T2DM pathogenesis, while providing an analytical blueprint for clinical translation of lipid mediator biomarkers in type 2 diabetic patients.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124871"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145621746","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"An optimized LC-ESI-MS/MS assay for erythrocyte 6-TG and 6-MMPD: Addressing critical methodological considerations for thiopurine metabolite monitoring","authors":"Ya-Min Chu ,&nbsp;Yuan-Yuan Zhang ,&nbsp;Ya-Hui Hu ,&nbsp;Jie Wang ,&nbsp;Hong-Li Guo ,&nbsp;Jin Xu ,&nbsp;Yong-Jun Fang ,&nbsp;Jing Xu ,&nbsp;Xuan-Sheng Ding ,&nbsp;Feng Chen","doi":"10.1016/j.jchromb.2025.124872","DOIUrl":"10.1016/j.jchromb.2025.124872","url":null,"abstract":"<div><div>Thiopurines, a class of antimetabolites widely used in patients with inflammatory bowel disease (IBD) and acute lymphoblastic leukemia (ALL), are associated with two predominant adverse effects: delayed myelotoxicity and hepatotoxicity. The erythrocyte-based active metabolites 6-thioguanine nucleotides (6-TGN) and 6-methylmercaptopurine nucleotides (6-MMPN) serve as biomarkers reflecting systemic drug exposure and predicting both therapeutic efficacy and adverse reactions. In this study, we successfully developed and validated a rapid, sensitive, and accurate liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) analytical method for simultaneous quantification of erythrocyte 6-TG and 6-MMPD concentrations. During method development and validation, we focused on addressing the following five key challenges currently of significant interest in the field: 1) Erythrocytes proved superior to whole blood as biological matrix; 2) Perchloric acid was essential in sample pretreatment; 3) Dual mobile phase additives (HCOOH+NH₄Ac) enhanced chromatographic peak shape and detection sensitivity; 4) Incomplete hydrolysis of 6-TGN and 6-MMPN occurred with heating durations &lt; 60 min; 5) The linear correlation coefficient of the 6-MMPD (6-MMP derivative, 4-amino-5-(methylthio)carbonyl imidazole) standard curve reflected the stable conversion efficiency of 6-MMP. The method exhibited excellent linearity over the concentration ranges of 0.06–50 μmol/L for 6-TG (<em>r</em> = 0.9906) and 0.18–150 μmol/L for 6-MMPD (<em>r</em> = 0.9914). Selectivity, carry-over, intra- and inter-batch accuracy and precision, reproducibility, recovery, matrix effect, and stability all complied with the acceptance criteria outlined in the US Food and Drug Administration (FDA) Bioanalytical Method Validation Guidance (2018). The validated method was successfully employed to quantify 6-TG and 6-MMPD in samples obtained from 20 patients with IBD or ALL.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124872"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145673397","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Recent advances in three-dimensional graphene and its derivatives for sample preparation in food contaminant analysis: A review","authors":"Xuesheng Zhou ,&nbsp;Fangyuan Li ,&nbsp;Kun Jiang ,&nbsp;Na Wang ,&nbsp;Bo Cui","doi":"10.1016/j.jchromb.2025.124862","DOIUrl":"10.1016/j.jchromb.2025.124862","url":null,"abstract":"<div><div>Due to their high specific surface area and extended π-conjugated systems, various three-dimensional graphene and its derivatives have been successfully synthesized and widely utilized for the enrichment of contaminants in food matrices. However, the diversity of synthetic approaches for these materials, coupled with their broad applicability in food contaminant extraction, has limited their effectiveness as a coherent and unified framework for guiding the development of detection methods. Therefore, it is assumed that a systematic review of these synthesis strategies, together with a comprehensive elucidation of the mechanisms underlying the extraction of various contaminants, would provide precise guidance for the design of detection methods based on such advanced materials. Based on this rationale, the review presents a systematic overview of the synthesis methods for three-dimensional graphene and its derivatives, accompanied by a critical evaluation of the advantages and limitations of each approach. Furthermore, it summarizes recent applications of these materials in the enrichment of diverse food contaminants and elucidates the underlying adsorption mechanisms. The results indicate that each synthetic method entails specific limitations: high energy consumption in hydrothermal and solvothermal methods, the use of toxic reagents in chemical reduction method, reliance on cross-linking agents in freeze-drying and three-dimensional printing techniques, and the requirement for sophisticated equipment in chemical vapor deposition. Nevertheless, integrating multiple approaches can effectively overcome the inherent drawbacks of individual methods, as demonstrated by the microwave-assisted hydrothermal method. Moreover, π–π stacking, hydrophobic, electrostatic interactions and hydrogen bonding collectively confer a distinct advantage in adsorption of aromatic food contaminants.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124862"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145578136","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Method development and validation for quantitative determination of urinary biomarkers of food intake for multiple foods","authors":"Christoph Hassenberg ,&nbsp;Sebastian T. Soukup ,&nbsp;Marina Armeni ,&nbsp;Achim Bub ,&nbsp;Jil V. Cannas ,&nbsp;David Fuentes ,&nbsp;Otto Savolainen ,&nbsp;Stephanie Seifert ,&nbsp;Rikard Landberg ,&nbsp;Sabine E. Kulling ,&nbsp;Carina I. Mack","doi":"10.1016/j.jchromb.2025.124793","DOIUrl":"10.1016/j.jchromb.2025.124793","url":null,"abstract":"<div><div>Biomarkers of food intake (BFIs) have emerged as a promising objective tool to complement traditional self-reported dietary assessment in nutritional research, with the potential to reduce systematic errors and improve accuracy. The development of comprehensive and robust quantification methods for BFIs is essential for widespread application. However, existing methods typically cover only a moderate number of BFIs per method, hindering their wide application in the field. In this study, we present the development and validation of a method for simultaneous quantification of 80 BFIs in urine reflecting 27 foods. The method utilizes a simple sample preparation procedure, followed by separation using both high-performance liquid chromatography (HPLC) on a C18 column and a hydrophilic interaction chromatography (HILIC) column, combined with tandem mass spectrometry in positive and negative mode (HPLC-MS/MS) (individual runs: 6 min). The working range for each analyte was determined in urine samples from a non-randomized, non-blinded nutritional intervention study. The method was validated with respect to selectivity, linearity, robustness, matrix effects, recovery, accuracy, and precision. In total, 44 BFIs could be absolutely quantified without or with only limitations at low concentrations, while 36 BFIs could only be measured semi-quantitatively, including 16 BFIs with limited validation data due to uncertainties. The 80 BFIs represent 27 foods (6 semi-quantitative) frequently consumed in European diets, including 24 plant-derived and 3 animal-derived items. The future implementation of this large-scale BFI quantification method in nutritional studies is expected to demonstrate the benefits of routinely measuring BFIs to improve the accuracy of dietary assessment.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1268 ","pages":"Article 124793"},"PeriodicalIF":2.8,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145415360","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A reversed-phase HPLC-based dual-parameter assay for the human urinary kallidinogenase enzyme activity","authors":"Hong-yan Ge ,&nbsp;Ya-jun Zhang ,&nbsp;Jun-qin Qiao ,&nbsp;Li Fan ,&nbsp;He-liang Fu ,&nbsp;Hong-zhen Lian","doi":"10.1016/j.jchromb.2025.124847","DOIUrl":"10.1016/j.jchromb.2025.124847","url":null,"abstract":"<div><div>In this work, a dual-parameter quantification protocol was successfully developed for determining the enzymatic activity of human urinary kallidinogenase (KN) using reversed-phase high-performance liquid chromatography (RP-HPLC). KN serves as a hydrolytic enzyme to cleave the substrate S-2266 (H-D-Val-Leu-Arg-pNA). Effective separation of the product, substrate, and KN was achieved under optimized chromatographic conditions. By minimizing matrix interference through HPLC separation and using multi-wavelength detection, both selectivity and sensitivity were significantly improved. Moreover, the dual-parameter quantification method, which simultaneously measured the formation of reaction products and the consumption of substrates to reflect KN enzyme activity, markedly improved the reliability of the determination. This method was successfully applied to the activity assay of actual KN samples. The established method has been demonstrated to be effective and reliable with comparable greenness. It provides a powerful tool for the quantitative monitoring of KN activity in biological products and paves the way for its application in complex biological matrices.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1268 ","pages":"Article 124847"},"PeriodicalIF":2.8,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145524977","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"γ-cyclodextrin based metal organic frameworks as micellar electrokinetic chromatography additive for the chiral separation of dansylated amino acids","authors":"Yan Zhang,&nbsp;Zexi Yu,&nbsp;Xiaotong Zhu,&nbsp;Rongyue Zhang,&nbsp;Nan Li,&nbsp;Min Wang,&nbsp;Juan Qiao","doi":"10.1016/j.jchromb.2025.124839","DOIUrl":"10.1016/j.jchromb.2025.124839","url":null,"abstract":"<div><div>A strategy utilizing oriented γ-cyclodextrin-based metal organic frameworks (γ-CD-MOFs) as chiral additives in micellar electrokinetic chromatography (MEKC) is presented for enhanced enantioseparation of dansylated D,L-amino acids (Dns-D,L-AAs). Its core innovation resides in the fixed orientation of γ-CD within the MOFs structure. This unique characteristic facilitates a shift in chiral recognition from “random interactions” to a “directional and highly efficient recognition” process, thereby substantially enhancing the resolution of chiral separation while overcoming the limitations of free γ-CD, including unstable interactions and poor reproducibility. Systematic optimization of SDS concentration (9.0 mM), γ-CD-MOFs concentration (16.0 mM), and buffer pH (9.5) yielded a maximum resolution (<em>R</em>_s) of 2.2, representing a 50 % improvement over traditional γ-CD. Under these conditions, 14 pairs of Dns-D,L-AAs achieved baseline separation, with 4 additional pairs showing partial separation. Quantitative validation for D,L-methionine (D,L-Met) demonstrated excellent linearity (19.8–1500 μM, r² = 0.999), low limits of detection (6.6 μM) and quantitation (19.8 μM), and high stability (relative standard deviations &lt;5 %). Application to rat plasma samples revealed peak concentration (C_max) of D,L-Met at 90 min post-injection, highlighting its utility in pharmacokinetic studies of amino acid-derived prodrugs (e.g., S-adenosylmethionine). This work introduces oriented γ-CD-MOFs as a transformative chiral additive in MEKC, offering superior selectivity and reproducibility for pharmaceutical and biomedical analyses.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1268 ","pages":"Article 124839"},"PeriodicalIF":2.8,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145415410","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Characterization and purification of hypoglycemic components from Rubus suavissimus leaf by affinity ultrafiltration, molecular docking, and macroporous resin","authors":"Xi Hu ,&nbsp;Siye Gao ,&nbsp;Hancong Wu ,&nbsp;Qingyun He ,&nbsp;Jianing Liu ,&nbsp;Danyue Zhao ,&nbsp;Zhenqiang Wu","doi":"10.1016/j.jchromb.2025.124830","DOIUrl":"10.1016/j.jchromb.2025.124830","url":null,"abstract":"<div><div>This study developed an environmentally friendly method for extracting polyphenols and rubusoside from <em>Rubus suavissimus</em> leaves. Under optimal extraction conditions, the contents of polyphenol and rubusoside reached 91.89 ± 2.39 mg/g and 47.03 ± 1.45 mg/g, respectively. The extract was purified by twelve types of macroporous resins, among which the ADS-7 resin had the highest static adsorption and desorption capacities. Optimized purification parameters for ADS-7 resin were determined by static and dynamic adsorption-desorption experiments and found to be: loading flow rate, 3 BV/h; loading concentration, 10 mg/mL; loading volume, 24 BV; elution solvent, 80 % (<em>v</em>/v) ethanol; elution speed, 3 BV/h; and elution volume, 20 BV. After purification, the content of polyphenols and rubusoside increased by 2.63 and 2.32 times, respectively. Kinetic and thermodynamic analyses revealed distinct adsorption mechanisms: polyphenols followed a pseudo-second-order model, whereas rubusoside followed a pseudo-first-order model; both exhibited spontaneous (ΔG &lt; 0) and endothermic (ΔH &gt; 0) physisorption.</div><div>Ultrafiltration-assisted centrifugal fractionation combined with UPLC-ESI-qTOF-MS/MS identified eight potential α-glucosidase inhibitors, including quercetin, apigenin, rutin, ellagic acid, kaempferol-3-O-rutinoside, kaempferol, rubusoside, and steviol. Molecular docking simulations revealed the molecular interactions between these compounds and α-glucosidase.</div><div>The enriched extract demonstrated enhanced bioactivity, with a 3.35-fold higher α-glucosidase inhibition, and its IC₅₀ values for DPPH and ABTS⁺ radical scavenging decreased from 142.03 μg/mL to 88.45 μg/mL and from 197.63 μg/mL to 107.63 μg/mL, respectively. These results substantiate the effectiveness of the extraction-purification approach for producing <em>R. suavissimus</em> leaf extracts and suggest their potential application as functional hypoglycemic and antioxidant food ingredients.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1268 ","pages":"Article 124830"},"PeriodicalIF":2.8,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145415411","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Causal effects of telomere length on ovarian tumor risk: Insights from genetic evidence","authors":"Tingyu Lang ,&nbsp;Xiaolei Liang ,&nbsp;Yongxiu Yang","doi":"10.1016/j.jchromb.2025.124845","DOIUrl":"10.1016/j.jchromb.2025.124845","url":null,"abstract":"<div><h3>Background</h3><div>Currently, contradictions remain regarding the causal relationship between telomere length (TL) and ovarian tumors (OT). To elucidate the potential causal relationship, we conducted a two-sample bidirectional Mendelian randomization (MR) study.</div></div><div><h3>Method</h3><div>All the data were from European populations and obtained from the Genome-Wide Association Study, the FinnGen study, and the Ovarian Cancer Association Consortium. We used inverse variance weighting (IVW) as the primary method, supplemented by other five methods to calculate odds ratios (OR) and 95 % confidence intervals (95 % CI) and checked for pleiotropy. Cochran's Q was used to detect heterogeneity.</div></div><div><h3>Results</h3><div>The IVW method supported TL as a risk factor for malignant (OR = 1.273, 95 % CI = 1.012–1.602) and benign ovarian tumors (BOTs) (OR = 1.337, 95 % CI = 1.093–1.637). Besides, ovarian cancer subtypes evaluated the strong causal relationship between TL and low malignant potential serous ovarian cancer (LMSOC) by applying the IVW method after Bonferroni correction. There was suggestive evidence for low malignant potential mucinous ovarian cancer, invasive mucinous ovarian cancer, and low-grade serous ovarian cancer. No causal relationships were found for other ovarian cancer subtypes.</div></div><div><h3>Conclusion</h3><div>Our MR study provides strong genetic evidence that longer telomere length increases risk of specific ovarian tumor subtypes—most robustly for benign ovarian tumors (BOTs) and low malignant potential serous ovarian cancer (LMSOC). For other subtypes, observed associations were suggestive but inconclusive after multiplicity correction, highlighting the etiological heterogeneity of ovarian tumors To optimize treatment regimens and preventive measures for OT, we will continue to thoroughly investigate the potential mechanism of action of these associations in future studies.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1268 ","pages":"Article 124845"},"PeriodicalIF":2.8,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145464641","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Bentonite modified with quaternary ammonium for enhanced human serum albumin adsorption","authors":"Saeed Barzegar ,&nbsp;Mehran Javanbakht ,&nbsp;Behrouz Akbari-Adergani","doi":"10.1016/j.jchromb.2025.124850","DOIUrl":"10.1016/j.jchromb.2025.124850","url":null,"abstract":"<div><div>Human Serum Albumin (HSA) is an important protein that helps regulate oncotic<!--> <!-->pressure and transport of diverse molecules. A high-performance adsorbent for the separation of albumin is strategic to improve efficiency and selectivity,<!--> <!-->which can result in a low-cost and simplified process for obtaining high-purity albumin. The present study aimed to elucidate the adsorption of HSA on modified bentonite and represent the adsorption capacity. Various characterizations confirm the modification and structural changes of bentonite after surface<!--> <!-->modification with dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride (DTSACL). A central composite design (CCD) for the response surface methodology (RSM) was used to investigate and optimize the effect of the pH, concentration of HSA, and sorbent dosage on the adsorption. The<!--> <!-->findings demonstrated that electrostatic interaction and functionalization of the surface were implemented to enhance the adsorption capacity of the modified bentonite. Thermodynamic investigations indicate an exothermic adsorption<!--> <!-->process and preferred ambient temperatures, while isothermal examinations confirm that monolayer adsorption was a better fit for the Langmuir model. The maximum adsorption capacity (q_e) of 430 mg /g was obtained with a desirability of 0.98 at optimized pH = 6.2,<!--> <!-->initial HSA concentration = 418.9 mg/L, and DTSACL-bentonite dosage = 30.1 mg in aqueous solution of HSA. The adsorption of HSA from real human serum samples achieved an adsorption efficiency of 79.8 % and a recovery rate of 92.5 %. High-performance liquid chromatography (HPLC) and SDS-PAGE analyses confirmed that DTSACL-bentonite exhibits high selectivity and efficiency, highlighting its potential as a promising adsorbent for the separation and purification of HSA.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1268 ","pages":"Article 124850"},"PeriodicalIF":2.8,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145524974","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Impact of Preprocessing and data analysis strategies on metabolite annotation in biological samples: A mass spectrometry-based metabolomics study using feature-based molecular networking","authors":"Qinyu Xiao ,&nbsp;Jiamin Yang ,&nbsp;Jianjun Xie ,&nbsp;Qing Liu ,&nbsp;Hongbo Huang ,&nbsp;Yiwen Tao ,&nbsp;Bo Ding","doi":"10.1016/j.jchromb.2025.124828","DOIUrl":"10.1016/j.jchromb.2025.124828","url":null,"abstract":"<div><div>Metabolomics workflows involve multiple complex steps including sample collection, storage, preparation, metabolite extraction, analytical platforms selection, data acquisition and interpretation. Each step may introduce variability that affects the quality and reliability of metabolomic data. To systematically investigate the effects of these factors on metabolomics outcomes, plasma samples from four different anatomical sites of colon cancer patients were analyzed using Liquid chromatography- Quadrupole-Exactive Orbitrap mass spectrometry (LC-Q-Exactive Orbitrap MS) for untargeted metabolomics. Response surface methodology was employed to optimize the ultrasound-assisted extraction conditions during sample pretreatment. Data analysis strategies were systematically evaluated, including Feature-Based Molecular Networking (FBMN) construction parameters and comparative assessment of different FBMN platforms for metabolite annotation. The optimized extraction conditions were determined as 300 % methanol concentration, sample freezing at −20 °C for 40 min, followed by ultrasonication for 5 min. Sample standardization protocols requiring single-use portioning and limiting freeze-thaw cycles to ≤2–3 cycles were identified as essential for reliable biomarker discovery and therapeutic mechanism exploration. Optimal FBMN construction parameters comprised a 25-min gradient elution time, 50 mm chromatographic column length, and high sample concentration. Comparative evaluation of Global Natural Products Social Molecular Networking (GNPS) and MZmine implementations of FBMN revealed that GNPS was recommended for studies prioritizing comprehensive annotation coverage and discovery-oriented metabolomics, while MZmine was preferred for method development, or applications requiring local processing without external data upload. This study demonstrated that preprocessing and data analysis strategies were critical determinants of data quality in untargeted plasma metabolomics. The findings provided evidence-based recommendations for experimental design, storage conditions, and data handling procedures that can guide protocol standardization and minimize undesired analytical variation in metabolomics studies.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1268 ","pages":"Article 124828"},"PeriodicalIF":2.8,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145415359","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}