Journal of Chromatography B最新文献

{"title":"Targeted mass spectrometry method for the determination of multiple gut-microbiota metabolites in human plasma","authors":"Sara R. Fernandes ,&nbsp;Cristian Azorín ,&nbsp;Eduarda M.P. Silva ,&nbsp;Manuel Miró ,&nbsp;Luisa Barreiros ,&nbsp;Marcela A. Segundo","doi":"10.1016/j.jchromb.2025.124764","DOIUrl":"10.1016/j.jchromb.2025.124764","url":null,"abstract":"<div><div>The gut microbiota profoundly impacts human health by producing metabolites that can act as biomarkers for disease diagnosis and therapy. However, accurately measuring these metabolites in biomatrices is challenging due to their low concentrations, high molecular diversity, and interference from matrix components, demanding advanced and precise analytical methodologies. Hence, an ultra-high-performance liquid chromatography method coupled to triple quadrupole-tandem mass spectrometry detection, combined with a chemical derivatization procedure, was developed and validated to quantify seven gut metabolites, namely acetic acid, propionic acid, butyric acid, <em>p</em>-cresol sulfate, 3-indoxyl sulfate, indole-3-acetic acid, and L-tryptophan, in human plasma. Samples were prepared by protein precipitation with acetonitrile and subsequently derivatized using 3-nitrophenylhydrazine. Chromatographic separation was achieved using a BEH C18 column, with elution performed at a flow rate of 0.2<!--> <!-->mL<!--> <!-->min⁻¹ and in gradient mode using formic acid-water (1:1000, <em>v</em>/<em>v</em>) and formic acid-acetonitrile (1:1000, <em>v</em>/<em>v</em>) as mobile phase components. The mass spectrometer was operated in negative ionization mode and data was acquired in selected reaction monitoring. Good linearity was achieved (<em>r</em>² &gt; 0.997) for all the target gut metabolites in the evaluated concentration ranges, with low LLOQ values (0.4–8 μM). The method proved to be accurate (87.0–114 %) and precise (CV ≤ 13.5 %), achieving a score of 65 in the Blue Applicability Grade Index (BAGI) metric, which confirmed its practicality. The developed method was ultimately employed to the analysis of plasma samples from children and adults involved in clinical studies, demonstrating its usefulness in medical research.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124764"},"PeriodicalIF":2.8,"publicationDate":"2025-08-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144885558","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":"Purification of steroidal saponins from dioscoreae hypoglaucae rhizoma by macroporous resin and evaluation of their anti-inflammatory effect","authors":"Zhangyi Qin ,&nbsp;Yifan Du ,&nbsp;Yue Zhong ,&nbsp;Ziyu Gu ,&nbsp;Qian Zheng ,&nbsp;Yuguang Zheng ,&nbsp;Dan Zhang ,&nbsp;Long Guo","doi":"10.1016/j.jchromb.2025.124769","DOIUrl":"10.1016/j.jchromb.2025.124769","url":null,"abstract":"<div><div>Dioscoreae hypoglaucae rhizome (DHR) is the dried rhizome of <em>Dioscorea hypoglauca</em> polibin, which is rich in steroidal saponins. The steroidal saponins present in DHR exhibit great pharmacological activities, particularly in inflammatory and anti-hyperuricemia effects. Despite steroidal saponins are recognized as primary bioactive components in DHR, the enrichment and purification processes of steroidal saponins is rare. The research aimed to explore the purification process and anti-inflammatory activity of steroidal saponins of DHR. Firstly, the steroidal saponins in DHR were characterized by UPLC-Q/TOF-MS, and six steroidal saponins including protodioscin, protogracillin, pseudoprotodioscin, pseudoprotogtacillin, dioscin and gracillin were initially identified. Then, the steroidal saponins in DHR were purified by seven types of macroporous resins (D-101, S-8, AB-8, ADS-7, HPD-600, HPD-100, DM130), and HPD-100 resin with relative great static adsorption and desorption capacities was used for purification of steroidal saponins from DHR. The optimized purification parameters of HPD-100 resin were explored by static and dynamic adsorption and desorption experiments, and optimal purification conditions were loading flow rate 1.2 BV/h, loading concentration 0.1 g/mL, loading volume 3.5 BV, elution solvent 70 % (<em>v</em>/v) ethanol, elution speed 1.2 BV/h and elution volume 3 BV. The purity of steroidal saponins was increased by 5.78 times (from 6.93 ± 0.01 % to 40.07 ± 2.63 %) after HPD-100 resin purification. Furthermore, the anti-inflammatory activities of the crude extracts and purified steroidal saponins extracts of DHR were investigated by LPS-stimulated RAW264.7 macrophages inflammation model. The results demonstrated the purified steroidal saponins extracts of DHR exhibited better anti-inflammatory activity compared to the crude extracts of DHR. This study conducted a feasible and efficient HPD-100 resin method for purification of steroidal saponins from DHR, and also provided evidences for the development and utilization of steroidal saponins in DHR.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124769"},"PeriodicalIF":2.8,"publicationDate":"2025-08-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144864126","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":"Utilizing liquid chromatography-mass spectrometry to map targeting of snake venom components by antivenom","authors":"Ramesh Kumar,&nbsp;Sunil Kumar,&nbsp;Anurag S. Rathore","doi":"10.1016/j.jchromb.2025.124768","DOIUrl":"10.1016/j.jchromb.2025.124768","url":null,"abstract":"<div><div>Preclinical efficacy testing is an essential aspect of evaluating quality of antivenoms (AVs). Recent years have witnessed a surge in development of in vitro methods to replace or reduce reliance on the standard mouse lethality assay. In this study, we propose a novel, reversed phase liquid chromatography-mass spectrometry (RPLC-MS)-based platform for monitoring AV activity on venom components under the WHO recommended in solution AV testing conditions. The method is simple and requires only 5 μg of venom and 389 μg AV for analysis. In addition to the identification and quantification of venom components that are effectively targeted by AV and those that are not, the MS coupling also enables, for the first time, the investigation of the impact of glycosylation – a post-translational modification (PTM) on AV activity. The ability of the platform to analyse intact toxins and facilitating direct comparison of peaks between the venom and the AV incubated samples allows for a simple MS1-based relative quantitation, circumventing the challenges associated with quantitation using bottom-up tandem MS studies for non-model organisms. Further, it also allows for quantitation of total antibodies in AV against individual toxins. The method also allows us to investigate time dependent AV activity, thus enabling studies of the kinetics of AV action on individual venom components. Venoms of Cobra and Russell's viper have been analyzed to demonstrate that the proposed LC-MS method offers a simple, specific, cost-effective, and quantitative approach for screening new or established antivenoms, paving the way for the next generation antivenomics.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124768"},"PeriodicalIF":2.8,"publicationDate":"2025-08-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144885560","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":"Development and validation of simultaneous quantification of total and free clozapine and its two metabolites in human plasma using ultra high-performance liquid chromatography coupled to tandem mass spectrometry","authors":"Rikako Kawanaka ,&nbsp;Takahiro Sumimoto ,&nbsp;Ryota Tanaka ,&nbsp;Toshihiko Izumi ,&nbsp;Moriaki Satoh ,&nbsp;Masaaki Muronaga ,&nbsp;Ryosuke Tatsuta ,&nbsp;Hirofumi Hirakawa ,&nbsp;Takeshi Terao ,&nbsp;Hiroki Itoh","doi":"10.1016/j.jchromb.2025.124763","DOIUrl":"10.1016/j.jchromb.2025.124763","url":null,"abstract":"<div><div>Several recent pharmacokinetic studies of clozapine (CLZ) and its metabolites have reported that plasma CLZ concentrations are associated with both efficacy and adverse effects, suggesting the usefulness of therapeutic drug monitoring. Although several quantification methods for total and free drug concentrations have been established, a simultaneous quantification method for total and free concentrations of CLZ and its metabolites using ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) has not been developed. In this study, we aimed to develop a simultaneous quantitative measurement method for wide ranges of plasma concentrations of total and free CLZ and its two major metabolites, <em>N</em>-desmethyl CLZ (NDC) and CLZ <em>N</em>-oxide (CNO), using UHPLC-MS/MS. Plasma samples were prepared by solid phase extraction, and the free fraction was obtained by ultrafiltration. This method meets the validation requirements of the U.S. Food and Drug Administration. The quantification method demonstrated good linearity over wide calibration ranges for total CLZ (10–1000 ng/mL), total NDC and CNO (40–4000 ng/mL), free CLZ (2–2000 ng/mL), and free NDC and CNO (0.8–800 ng/mL). Ultrafiltration recovery rates for free CLZ, NDC, and CNO were approximately 60.0 %, 65.4 %, and 72.8 %, respectively. The total drug recovery rates ranged from 91.4 % to 107.5 %, and the free drug recovery rates ranged from 88.5 % to 117.1 %. Furthermore, we successfully measured total and free CLZ, NDC, and CNO concentrations in plasma samples of 12 patients with schizophrenia treated with CLZ. We have successfully developed and validated a method for quantitative measurement of total and free CLZ, NDC, and CNO concentrations in plasma.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124763"},"PeriodicalIF":2.8,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144841298","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":"Spectrum-effect relationship between HPLC fingerprints and antitumor activities of Inonotus hispidus","authors":"Changsong Xu ,&nbsp;Hongyu Niu ,&nbsp;Xinghao Liu ,&nbsp;Xiuqiang Xia ,&nbsp;Guoying Zhang ,&nbsp;Fengjun Liu ,&nbsp;Jianya Ling","doi":"10.1016/j.jchromb.2025.124766","DOIUrl":"10.1016/j.jchromb.2025.124766","url":null,"abstract":"<div><div><em>Inonotus hispidus</em> (<em>I. hispidus</em>), a traditional edible and medicinal fungus, has been widely used in the fields of medicine and health care. Modern pharmacological studies have confirmed that this fungus exhibits various biological activities, including antitumor, antioxidant, and hypoglycemic effects. However, the underlying mechanisms linking its antitumor activity to specific chemical constituents have not yet been fully elucidated. In this study, HPLC fingerprints of 11 batches of <em>I. hispidus</em> were established. The inhibitory effects of these samples on 4 T1 and HeLa cells were evaluated using the MTT assay. The correlation between the HPLC fingerprints and antitumor activity was analyzed using grey relational analysis and partial least squares regression. The results indicated that the antitumor activity of <em>I. hispidus</em> was due to the synergistic effects of multiple components. Of these, peaks 3, 5 (hispidin), 6, and 7 were identified as key contributors. Notably, these key components were predominantly enriched in the ethyl acetate fraction. The accuracy of the correlation results was validated by performing in vitro inhibition of 4 T1 cell viability using different extraction solvents. This study provides scientific evidence for the antitumor potential of <em>I. hispidus</em> and helps clarify the spectrum–effect relationship of its active components</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124766"},"PeriodicalIF":2.8,"publicationDate":"2025-08-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144830907","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":"Network pharmacology and untargeted metabolomics reveal the mechanisms of Bushen Kaixuan Tongluo formula in diabetic kidney disease","authors":"You Wang ,&nbsp;Baosheng Zhao ,&nbsp;Zhuqing Yang ,&nbsp;Lingling Qin ,&nbsp;Haiyan Wang ,&nbsp;Cuiyan Lv ,&nbsp;Tonghua Liu ,&nbsp;Guangrui Huang","doi":"10.1016/j.jchromb.2025.124752","DOIUrl":"10.1016/j.jchromb.2025.124752","url":null,"abstract":"<div><div>Bushen Kaixuan Tongluo Formula (BKT), a clinically validated Traditional Chinese Medicine, has shown promising renoprotective effects in diabetic kidney disease (DKD) patients. This study investigated the therapeutic mechanisms of BKT in DKD using an integrated approach combining network pharmacology and untargeted metabolomics in db/db mice. Network pharmacology identified 338 bioactive components in BKT targeting 389 DKD-related genes, with key pathways including AGE-RAGE, HIF-1, MAPK, and PI3K-Akt signaling, as well as autophagy. BKT treatment significantly improved renal function (reduced ACR), ameliorated glucose/lipid metabolism (lowered GSP, INS, HOMA-IR, TC, FFA), and attenuated renal pathology (reduced glomerulosclerosis, tubular injury, and fibrosis). Untargeted metabolomics revealed 26 renal and 28 urinary differential metabolites (VIP &gt; 1.0, <em>P</em> &lt; 0.05), with enrichment in autophagy, PPAR signaling, linoleic acid metabolism (kidney), and TCA cycle/thiamine metabolism (urine). Key metabolites such as α-dimorphecolic acid (renal), thiamine pyrophosphate (urinary), and LysoPC (18:4) were implicated in BKT's renoprotective effects. These findings demonstrate that BKT alleviates DKD through multi-target modulation of metabolic, inflammatory, and stress-response pathways, with synergistic actions predicted by network pharmacology and validated by metabolomics. This study provides a scientific foundation for clinical application of BKT in DKD treatment.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124752"},"PeriodicalIF":2.8,"publicationDate":"2025-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144841297","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":"Development and validation of a ‘dilute and shoot’ LC–MS/MS method in urine suitable for screening and confirmation analyses in a clinical setting","authors":"Dimitra Florou ,&nbsp;Amvrosios Orfanidis ,&nbsp;Vassiliki A. Boumba","doi":"10.1016/j.jchromb.2025.124750","DOIUrl":"10.1016/j.jchromb.2025.124750","url":null,"abstract":"<div><div>Urine toxicological analysis serves as a significant tool in both clinical and forensic contexts, facilitating the diagnosis of acute intoxications, determination of causes of death, monitoring of substance use in occupational settings, and identification of drug-facilitated crimes. In this regard, the dilute-and-shoot method, when integrated with liquid chromatography-tandem mass spectrometry (LC–MS/MS), represents a promising analytical approach due to its efficacy, reliability, and wide-ranging applicability. This study presents the development and validation of an LC–MS/MS method that simultaneously detects and quantitates 115 drugs and metabolites comprising analytes from different categories, such as drugs of abuse (DOA), new psychoactive substances (NPS), prescription and over-the-counter drugs. Sample pretreatment was studied by applying different solvents (acetonitrile, water or methanol), and the best results were obtained after adding 100 μL of sample, 200 μL of a mixture of methanol: acetonitrile (3:1, <em>v</em>/v). The mixture was vortexed, centrifuged and the supernatant directly injected into the instrument. The analysis took place on a C18 column with a gradient elution over 7.5 min. The method was found to be selective and sensitive, offering LOD/LOQ ranging from 0.01 to 1.5/ 0.05–5 ng/mL, respectively. Validation of the method included evaluation of recovery, carryover, matrix effect, accuracy, precision, selectivity, stability and dilution integrity. The method performed satisfactorily and was therefore applied to urine samples that collected over a 12-week period from individuals enrolled in a rehabilitation program. The proposed method was applied as a follow-up tool aiming to detect prescribed (or not) medicine, as well as other illegal substances.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124750"},"PeriodicalIF":2.8,"publicationDate":"2025-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144809359","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":"Analysis of lipid nanoparticles using two-dimensional chromatography: Simultaneous determination of encapsulation efficiency, nucleic acid integrity, and size of LNP formulations","authors":"Nejc Pavlin,&nbsp;Mojca Bavčar,&nbsp;Tristan Kovačič,&nbsp;Tjaša Kašček,&nbsp;Anže Martinčič Celjar,&nbsp;Ines Bergoč,&nbsp;Andreja Gramc Livk,&nbsp;Aleš Štrancar","doi":"10.1016/j.jchromb.2025.124751","DOIUrl":"10.1016/j.jchromb.2025.124751","url":null,"abstract":"<div><div>Lipid nanoparticles (LNPs) have emerged as the most advanced drug delivery system for gene therapies and vaccines due to their ability to encapsulate a diverse range of payloads, including nucleic acids and proteins. LNPs provide many benefits, such as protection of payloads from enzymatic degradation, enhanced cellular uptake, and controlled release, making them promising candidates for therapeutic applications. The complex composition and inherent instabilities of LNPs present significant challenges for their characterization, especially in determining encapsulation efficiency, payload integrity, and size distribution. This study presents a two-dimensional chromatography (2D) method to simultaneously assess crucial parameters of LNP formulations. The method employs a switching chromatography system comprising two distinct analytical columns, independent pumps, and two detectors, including an ultraviolet-visible detector (UV–Vis) and a multi-angle light scattering detector (MALS). A key benefit of this advanced configuration is the direct analysis of LNPs without the need for sample preparation. The 2D technique enables accurate quantification of both encapsulated and non-encapsulated nucleic acids, evaluation of payload integrity, and determination of LNP size and size distribution. The results demonstrate that this method provides a comprehensive and robust analytical solution, enabling further development and understanding of lipid-based drug delivery systems. The validation of the technique confirms its sensitivity (LOD 15 ng mRNA, LOQ 45 ng mRNA), linearity (R² &gt; 0.99), precision (RSD &lt; 15 %), accuracy (&lt; 15 %), and potential to streamline and optimize process development, in-process control, and quality control of LNP formulations.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124751"},"PeriodicalIF":2.8,"publicationDate":"2025-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144809360","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":"Development of an alternative method for purification and kinetic properties of polyphenol oxidase from some apple cultivars","authors":"Esra Dereli,&nbsp;Dudu Demir","doi":"10.1016/j.jchromb.2025.124745","DOIUrl":"10.1016/j.jchromb.2025.124745","url":null,"abstract":"<div><div>In this study, an alternative method to purify the polyphenol oxidase (PPO) was developed. For this purpose, a novel affinity gel was synthesized by first Sepharose-4B being activated by cyanogen bromide (CNBr), then L-tyrosine (as a spacer arm) was coupled to CNBr-activated Sepharose-4B, and then <em>o</em>-aminobenzoic acid, as a ligand for purification of the PPO, was coupled to L-tyrosine. PPO enzymes were purified from Starking Delicious, Granny Smith, and Golden Delicious apple cultivars grown in the Eğirdir district of Isparta/Türkiye by utilizing both the Sepharose 4B-L-tyrosine-<em>p</em>-aminobenzoic acid affinity gel and the novel affinity gel. 101.59, 22.69, and 12.81 purification folds were achieved from Starking Delicious, Granny Smith, and Golden Delicious cultivars, respectively, by using the novel gel. 128.95, 25.60, and 45.92 purification folds were achieved in the Starking Delicious, Granny Smith, and Golden Delicious cultivars, respectively, by utilizing Sepharose 4B-L-tyrosine-<em>p</em>-aminobenzoic acid. The <em>K</em><em>m</em>, <em>Vmax</em>, and <em>Vmax</em>/<em>K</em><em>m</em> values were calculated to be 20 mM, 25,000 U/mLmin, and 1,250 U/mLminmM; 40 mM, 20,000 U/mLmin, and 500 U/mLminmM; and 50 mM, 5,000 U/mLmin, and 100 U/mLminmM for the purified PPO enzymes of the Starking Delicious, Granny Smith, and Golden Delicious cultivars, respectively, by using catechol as substrate by the Lineweaver-Burk method. This study investigated the effect of para and ortho substituent positioning on ligand performance in affinity chromatography purification. The findings show that a novel affinity gel using an <em>o</em>-aminobenzoic acid ligand is effective for PPO purification, highlights the importance of ligand structure in affinity chromatography, and contributes significantly to enzyme purification.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1265 ","pages":"Article 124745"},"PeriodicalIF":2.8,"publicationDate":"2025-07-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144781408","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":"One-step synthesis of high-hydrophilic hydrothermal spheres for N-glycosylated peptides and exosomes analysis in diabetes serum","authors":"Yi Yan ,&nbsp;Zifang Peng ,&nbsp;Luyan Meng ,&nbsp;Wenfen Zhang ,&nbsp;Chuan-Fan Ding ,&nbsp;Shusheng Zhang","doi":"10.1016/j.jchromb.2025.124748","DOIUrl":"10.1016/j.jchromb.2025.124748","url":null,"abstract":"<div><div>Clarifying the pathogenesis of diabetes contributes to prevent the occurrence of diabetes. Glycosylated proteins carried by serum exosomes are possibly used as biomarkers of some diseases. In this work, a novel hydrophilic carbonaceous sphere was prepared via one-step hydrothermal carbonization (HTC) process by using glucose as raw material, 1,2-epoxy-5-hexene as a linker, 2-aminopurine as hydrophilic functional group, water as the sole solvent (denoted as CS@2AP). The synthesis process was simple and eco-friendly. The obtained CS@2AP proposed high sensitivity (0.08 fmol μL⁻¹) and excellent selectivity (1:1000) for glycopeptides enrichment. Moreover, CS@2AP displayed good isolation effect for serum exosomes from diabetes patient analyzed by western blot. Furthermore, when CS@2AP was used for glycopeptides analysis from exosome digests, 68 glycopeptides were specifically captured.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124748"},"PeriodicalIF":2.8,"publicationDate":"2025-07-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144723700","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}