Journal of Chromatography B最新文献_第4页

LC-MS/MS analysis of five antibiotics in dried blood spots for therapeutic drug monitoring of ICU patients LC-MS/MS分析5种抗生素用于ICU患者治疗药物监测

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-06-07 DOI: 10.1016/j.jchromb.2025.124699

Zhan Qi, Sha Zhang, Jie Li, Shijing Qian, Danfei Song, Xiancheng Ye

{"title":"LC-MS/MS analysis of five antibiotics in dried blood spots for therapeutic drug monitoring of ICU patients","authors":"Zhan Qi, Sha Zhang, Jie Li, Shijing Qian, Danfei Song, Xiancheng Ye","doi":"10.1016/j.jchromb.2025.124699","DOIUrl":"10.1016/j.jchromb.2025.124699","url":null,"abstract":"<div><div>In the intensive care unit (ICU), optimizing antimicrobial therapy through Therapeutic Drug Monitoring (TDM) can significantly improve patient outcomes. We developed and validated a DBS method for the simultaneous quantification of five antibiotics commonly used in ICUs, namely imipenem, meropenem, tigecycline, teicoplanin, and vancomycin. Dried blood spots (DBS) were prepared by spotting 30 μL of blood onto Whatman 903® cards and analyzed using ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). The DBS concentrations measured were compared with serum concentrations analyzed using standard laboratory methods. The paired DBS and serum samples were obtained from ICU. Deming regression and Bland-Altman difference plot were used to assess the consistency between the two methods. The DBS method was validated including selectivity, carryover, precision (0.078–16.70 %), accuracy (85.19–117.17 %), matrix effect, recovery (46.51 %–114.15 %), linearity, and dilution integrity. DBS samples stability at −80 °C for at least 30 days. DBS and serum concentrations of two antibiotics were compared, and statistical analysis confirmed good correlation (<em>r</em> > 0.97) between them. This study provides a new approach to TDM, suggesting that DBS may replace or complement traditional analytical sampling techniques. It has been validated for guiding individualized antimicrobial therapy in ICU patients.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124699"},"PeriodicalIF":2.8,"publicationDate":"2025-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144290581","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}

引用次数: 0

Absolute quantitative lipidomics of Clonorchis sinensis-infected rats reveals key alterations in metabolic pathways 华支睾吸虫感染大鼠的绝对定量脂质组学揭示了代谢途径的关键改变

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-06-06 DOI: 10.1016/j.jchromb.2025.124672

Zhenli Xu , Shiwen Hua , Jian Ding , Xinyi Hu , Rui Chen , Yang Cheng , Su Han

{"title":"Absolute quantitative lipidomics of Clonorchis sinensis-infected rats reveals key alterations in metabolic pathways","authors":"Zhenli Xu , Shiwen Hua , Jian Ding , Xinyi Hu , Rui Chen , Yang Cheng , Su Han","doi":"10.1016/j.jchromb.2025.124672","DOIUrl":"10.1016/j.jchromb.2025.124672","url":null,"abstract":"<div><div><em>Clonorchis sinensis</em> (<em>C. sinensis</em>) infection is a significant public health concern due to its association with chronic hepatobiliary diseases. However, the mechanisms underlying <em>C. sinensis</em> infection and its effects on host metabolism remain poorly understood. In this study, serum samples were collected from rats at 4 and 8 weeks post-infection (wpi), and lipid metabolites were analyzed using absolute quantitative lipidomics with UHPLC-MS/MS. Multivariate analyses were conducted to identify differentially expressed lipids, and pathway analysis was performed utilizing the MetaboAnalyst and KEGG databases.</div><div>A total of 12 lipid subclasses across five major categories were identified, with triacylglycerols (TAG) being the most significantly affected. At 4 wpi, 230 lipids were up-regulated and 18 down-regulated, whereas at 8 wpi, 88 were up-regulated and 73 down-regulated compared to controls. The results revealed significant alterations in lipid profiles, particularly in TAG, free fatty acids (FFA), and phosphatidylcholine (PC), with phosphatidylethanolamine (PE) exhibiting the most pronounced dynamic changes. Pathway enrichment analysis revealed significant involvement of the biosynthesis of unsaturated fatty acids, alpha-linolenic acid metabolism, and glycerolipid metabolism in response to the infection.</div><div>This study identifies significant alterations in the lipidomics of <em>C. sinensis</em>-infected rats, revealing critical perturbations in key metabolic pathways, which are likely involved in the host's immune and inflammatory responses. These findings not only offer potential therapeutic targets, but also deepen our understanding of host-parasite metabolic interactions during chronic infection.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124672"},"PeriodicalIF":2.8,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144271052","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}

引用次数: 0

Quantification of amikacin, gentamicin, and tobramycin in capillary plasma microsamples by LC-MS/MS LC-MS/MS定量毛细管血浆微量样品中阿米卡星、庆大霉素和妥布霉素的含量

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-06-06 DOI: 10.1016/j.jchromb.2025.124698

Ana Paula Grando , Ana Carolina Fritsch , Amanda Pacheco Bondan , Carolina Weber Ferrareze , Giovana Piva Peteffi , Roberta Zilles Hahn , Ana Júlia Dossena , Juliana Raquel Raasch , Marina Venzon Antunes , Rafael Linden

{"title":"Quantification of amikacin, gentamicin, and tobramycin in capillary plasma microsamples by LC-MS/MS","authors":"Ana Paula Grando , Ana Carolina Fritsch , Amanda Pacheco Bondan , Carolina Weber Ferrareze , Giovana Piva Peteffi , Roberta Zilles Hahn , Ana Júlia Dossena , Juliana Raquel Raasch , Marina Venzon Antunes , Rafael Linden","doi":"10.1016/j.jchromb.2025.124698","DOIUrl":"10.1016/j.jchromb.2025.124698","url":null,"abstract":"<div><div>Aminoglycoside antibiotics, including amikacin (AMI), gentamicin (GEN), and tobramycin (TOB), are widely used to treat infections, necessitating plasma concentration monitoring to achieve therapeutic targets and optimize patient treatment. To minimize patient discomfort, less invasive blood collection methods are desirable. Capillary blood microsampling provides an alternative to conventional venous collection, enabling the extraction of small plasma volumes via distal puncture or self-lancing devices. This study developed and validated an LC-MS/MS method for quantifying AMI, GEN, and TOB in plasma microsamples, comparing concentrations obtained from venous and capillary plasma. Capillary samples were collected using the TASSO<sup>+</sup>® device or heparinized glass capillaries. The method was validated according to ICH guidelines, demonstrating linearity of 0.5–50 mg/L for GEN and 1.0–100 mg/L for AMI and TOB, with extraction efficiencies exceeding 85 % for all analytes. Accuracy ranged from 94.9 % to 108.1 %, with precision between 1.04 % and 5.62 %, and matrix effects of 5.5 % to 20.5 %. A total of 23 paired venous and capillary plasma samples were analyzed, with Passing-Bablok regression revealing strong agreement between venous and capillary plasma concentrations for AMI (<em>r</em> = 0.980, <em>P</em> < 0.0001) and GEN (<em>r</em> = 0.979, <em>P</em> < 0.0001). These findings suggest that capillary microsampling is a viable and clinically applicable alternative for therapeutic drug monitoring of aminoglycosides.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124698"},"PeriodicalIF":2.8,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144241414","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}

引用次数: 0

Xuefu Zhuyu decoction ameliorates atherosclerosis in ApoE−/− mice by regulating cholesterol metabolism and inflammation 血附竹骨汤通过调节胆固醇代谢和炎症改善ApoE−/−小鼠动脉粥样硬化

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-06-04 DOI: 10.1016/j.jchromb.2025.124693

Yaobin Zhu , Yonghao Chen , Ruxi Tong , Xuanbin Huang , Bilin Xu , Jinshui Chen , Tianmin Wu

{"title":"Xuefu Zhuyu decoction ameliorates atherosclerosis in ApoE−/− mice by regulating cholesterol metabolism and inflammation","authors":"Yaobin Zhu , Yonghao Chen , Ruxi Tong , Xuanbin Huang , Bilin Xu , Jinshui Chen , Tianmin Wu","doi":"10.1016/j.jchromb.2025.124693","DOIUrl":"10.1016/j.jchromb.2025.124693","url":null,"abstract":"<div><h3>Objective</h3><div>This study endeavors to investigate the effect of Xuefu Zhuyu decoction (XFZY) on atherosclerosis in ApoE<sup>−/−</sup> mice fed with a high-fat diet, as well as the latent molecular mechanisms involved.</div></div><div><h3>Methods</h3><div>ApoE<sup>−/−</sup> mice were fed a 40 % high-fat diet to induce atherosclerotic phenotype. Standard diet syngeneic C57BL/6 mice of the same age were used for the control group. The drug-treated groups received high-dose and low-dose XFZY via continuous intragastric administration in atherosclerotic mice. The concentrations of the inflammatory factors were measured. The lipid deposition, pathological changes and collagen expression in the thoracic aorta wall were detected. The levels of expression of CD36, ABCA1, SR-A1, and ABCG1 were quantified within the thoracic aorta tissue.</div></div><div><h3>Results</h3><div>In the XFZY-treated group, a notable decline was observed in serum lipid levels, as well as in the concentrations of inflammatory factors. This reduction was accompanied by a decrease in the accumulation of lipids within the wall of the thoracic aorta. The XFZY treatment leaded in a decrease in the expression value of collagen I and III within the thoracic aorta. Pathological examination of the thoracic aorta indicated alleviation of atherosclerotic lesions. Intriguingly, The study observed a downregulation of SR-A1 and CD36 expression, accompanied by an upregulation of ABCG1 and ABCA1 in atherosclerosis-induced mice models.</div></div><div><h3>Conclusion</h3><div>XFZY exerts an anti-atherosclerotic effect not only by reducing serum lipid and inflammatory levels but also by decreasing thoracic aortic lipid deposition, repairing endothelial injury, and stabilizing atherosclerotic plaques. The underlying process might deal with an augmentation in cholesterol efflux and the facilitation of reverse cholesterol transport.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124693"},"PeriodicalIF":2.8,"publicationDate":"2025-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144232610","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}

引用次数: 0

Simulation of sildenafil metabolism using an electrochemical oxidation system 电化学氧化系统模拟西地那非的代谢

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-06-04 DOI: 10.1016/j.jchromb.2025.124695

Unyong Kim , Sumin Seo , Jiyu Kim , Chohee Jeong , Woojin Jeong , Han Young Eom , Joon Hyuk Suh , Junghyun Kim , Hyun-Deok Cho , Sang Beom Han

{"title":"Simulation of sildenafil metabolism using an electrochemical oxidation system","authors":"Unyong Kim , Sumin Seo , Jiyu Kim , Chohee Jeong , Woojin Jeong , Han Young Eom , Joon Hyuk Suh , Junghyun Kim , Hyun-Deok Cho , Sang Beom Han","doi":"10.1016/j.jchromb.2025.124695","DOIUrl":"10.1016/j.jchromb.2025.124695","url":null,"abstract":"<div><div>Drug metabolism studies play a pivotal role in drug development, as they help predict the toxicity of newly developed drugs. Traditional approaches for drug metabolism studies often utilize cytochrome P450 systems, such as liver microsomes and hepatocytes. Recently, electrochemical oxidation systems have emerged as a promising alternative, capable of simulating phase I metabolic reactions, including hydroxylation, <em>N</em>-dealkyation, <em>S</em>-oxidation, <em>P</em>-oxidation, and dehydrogenation. Additionally, mass spectrometry (MS) has become indispensable in drug metabolism research due to its ability to detect trace amounts of metabolites and elucidate the structures of unknown metabolites using tandem MS spectra. In this study, we simulated sildenafil metabolism using an electrochemical oxidation system. The similarity between metabolic profiles generated by the electrochemical oxidation system and the liver microsomal incubation system was assessed using Pearson's correlation coefficient. A total of 96 metabolites and oxidation products were detected in both systems. Among the tested conditions, the profile of oxidation products generated at the glassy carbon electrode (ammonium acetate, pH 8.0) showed the highest correlation with the metabolic profile from the human liver microsome system at 25 μmol/L of sildenafil, highlighting the ability of this electrochemical setup to effectively mimic in vitro microsomal metabolism. In conclusion, while electrochemical oxidation systems cannot entirely replace traditional in vitro metabolism models, such as liver microsomes, S9 fractions, and hepatocytes, these findings highlight the importance of EC systems as complementary tools in metabolic studies, opening new avenues for progress in drug metabolism research.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124695"},"PeriodicalIF":2.8,"publicationDate":"2025-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144280314","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}

引用次数: 0

Preparation of molecularly imprinted polymers for the selective extraction and purification of hesperidin from orange peels 分子印迹聚合物的制备及其对橙皮中橙皮苷的选择性提取和纯化

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-06-04 DOI: 10.1016/j.jchromb.2025.124696

Qiurui Zhao , Xinyao Yu , Mengyuan Liu , Chuansen Qin , Yahui He , Suilou Wang , Haixiang Wang

{"title":"Preparation of molecularly imprinted polymers for the selective extraction and purification of hesperidin from orange peels","authors":"Qiurui Zhao , Xinyao Yu , Mengyuan Liu , Chuansen Qin , Yahui He , Suilou Wang , Haixiang Wang","doi":"10.1016/j.jchromb.2025.124696","DOIUrl":"10.1016/j.jchromb.2025.124696","url":null,"abstract":"<div><div>Orange peels are a common by-product in the global food processing industry, leading to resource wastage and environmental pollution. They are rich in hesperidin, a flavonoid with multiple pharmacological and biological activities, possessing significant economic value. Based on this, in this study, a one-pot method was developed to create hesperidin MIPs for selective separation and purification of hesperidin from waste orange peels. To obtain the optimal MIPs, the best functional monomer was first determined through computer simulations and spectroscopic scanning, and the synthesis process was optimized. The characterization results demonstrated that the obtained MIPs, due to the presence of the functional monomer 2-vinylpyridine (2-VP), effectively adsorbs hesperidin through hydrophobic interactions and π-π stacking between the benzene ring and pyridine ring, achieving an adsorption capacity of 74.18 mg/g. MIPs exhibited excellent selectivity in the presence of two structural analogs, naringin and neohesperidin, and the imprinting factor reached 2.01. Furthermore, the MIPs exhibited excellent selectivity in the presence of structurally similar compounds within a complex matrix. In practical applications using MIPs as the adsorbent, the maximum extraction efficiency of hesperidin can reach 73.88 %, with the purity of extracted hesperidin reaching 81.24 %. After seven consecutive adsorption-desorption cycles, the adsorption capacity of MIPs for hesperidin decreased by only 1.55 mg/g. This research provides a simple and efficient integrated strategy for the separation and purification of hesperidin from orange peel waste, with great potential for commercial application.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124696"},"PeriodicalIF":2.8,"publicationDate":"2025-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144241413","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}

引用次数: 0

Development and validation of a high-throughput LC-MS/MS bioanalytical method for the simultaneous quantification of cannabidiol and metabolites in human plasma. 同时定量人血浆中大麻二酚及其代谢物的高通量LC-MS/MS生物分析方法的建立和验证。

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-06-03 DOI: 10.1016/j.jchromb.2025.124694

Ryan De Palma, Murali K. Matta, Vikram Patel, Jeffry Florian, David G. Strauss, Rodney Rouse

{"title":"Development and validation of a high-throughput LC-MS/MS bioanalytical method for the simultaneous quantification of cannabidiol and metabolites in human plasma.","authors":"Ryan De Palma, Murali K. Matta, Vikram Patel, Jeffry Florian, David G. Strauss, Rodney Rouse","doi":"10.1016/j.jchromb.2025.124694","DOIUrl":"10.1016/j.jchromb.2025.124694","url":null,"abstract":"<div><div>The removal of hemp from the definition of marijuana in the 2018 Agricultural Improvement Act has increased the number of cannabidiol-containing products available to consumers. Consequently, consumer use has also increased. Increased product availability and use drives the need for sensitive and specific analytical assays to measure the cannabidiol (CBD) and metabolites in patients, to establish dose–effect relationships and to gain knowledge of their pharmacokinetics. Here we describe the development and validation of a rapid high-throughput LC-MS/MS bioanalytical method for the quantification of cannabidiol and primary metabolites in human plasma to support an FDA-sponsored clinical study (<span><span>NCT06192589</span><svg><path></path></svg></span>). Sample preparation a single step protein precipitation followed by filtration through 96-well Phree™ Phospholipid removal plates. The method was validated over ranges of CBD: 1.95–500.00 ng mL<sup>−1</sup>; 7-hydroxy-cannabidiol (7-OH-CBD): 3.91–1000.00 ng mL<sup>−1</sup>; 7-carboxy-cannabidiol (7-COOH-CBD): 31.25–8000.00 ng mL<sup>−1</sup>. There was no cross-analyte interference, injection carryover, or matrix effect observed with this method. Analyte recoveries were consistent across three QC levels ranging from 83.90 to 90.85 %. Inter-day Accuracy across four QC level of all three analytes ranged from 93.87 to 107.31 % while precision ranged from 1.03 to 14.33 %. These results and other outlined in this manuscript met acceptance criteria as outline the current M10 Guidance for Bioanalytical Method Validation and Study Sample Analysis.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124694"},"PeriodicalIF":2.8,"publicationDate":"2025-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144221831","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}

引用次数: 0

Analysis of Angelica sinensis at different growth stages by 1H NMR-based metabolic fingerprinting combined with chemometrics 基于1H核磁共振代谢指纹图谱结合化学计量学分析当归不同生长期

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-05-29 DOI: 10.1016/j.jchromb.2025.124676

Xinbo Pan , Zhirong Gu , Yingwen Yang , Rina Sa , Yali Wang

{"title":"Analysis of Angelica sinensis at different growth stages by 1H NMR-based metabolic fingerprinting combined with chemometrics","authors":"Xinbo Pan , Zhirong Gu , Yingwen Yang , Rina Sa , Yali Wang","doi":"10.1016/j.jchromb.2025.124676","DOIUrl":"10.1016/j.jchromb.2025.124676","url":null,"abstract":"<div><div>The metabolite fingerprint analysis was performed using <sup>1</sup>H NMR spectroscopy was adopted for systematically evaluate the <em>Angelica sinensis</em> metabolite profile analysis in diverse growth periods, along with the identification of the metabolites, so as to analyze changes in <em>Angelica sinensis</em> secondary metabolites during growth. This aims at analyzing changes in <em>Angelica sinensis</em> secondary metabolites during growth. Metabolic profiles were analyzed through <sup>1</sup>H NMR spectroscopy, meanwhile, crude extracts in the root of <em>Angelica sinensis</em> were analyzed in terms of multivariate data. <sup>1</sup>H NMR chemical shifts were compared with those of available reference standards to identify metabolites. Principal component analyses (PCA) together with partial least-squares discriminate analysis (PLS-DA) on <sup>1</sup>H NMR data clearly separated different year's samples by components axis. According to this study, <em>Angelica sinensis</em> secondary metabolite accumulation was tightly associated with growth periods, demonstrating that metabolomics might be used in the natural health product <em>Angelica sinensis</em>. The <sup>1</sup>H NMR-based metabolomics technology may be used to explore changes in <em>Angelica sinensis</em> secondary metabolites in the process of growth. As revealed by <sup>1</sup>H NMR metabolite fingerprinting in combination with chemometric analysis, some substances like ferulic acid, ligustilide, levistilide A and sugars could be quality assurance markers for <em>Angelica sinensis</em>.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124676"},"PeriodicalIF":2.8,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144195311","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}

引用次数: 0

Hollow polymer nanospheres (HPSs) as reusable adsorbent for solid-phase extraction (SPE) of trans, trans-muconic acid from urine samples 中空聚合物纳米球（hps）作为固相萃取（SPE）尿液中反式、反式粘膜酸的可重复使用吸附剂

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-05-28 DOI: 10.1016/j.jchromb.2025.124674

Nematullah Kurd , Abbas Afkhami , Hanieh Ganji

{"title":"Hollow polymer nanospheres (HPSs) as reusable adsorbent for solid-phase extraction (SPE) of trans, trans-muconic acid from urine samples","authors":"Nematullah Kurd , Abbas Afkhami , Hanieh Ganji","doi":"10.1016/j.jchromb.2025.124674","DOIUrl":"10.1016/j.jchromb.2025.124674","url":null,"abstract":"<div><div>In the present work, hollow polymer nanospheres (HPSs) were prepared and applied as reusable adsorbent in solid-phase extraction (SPE) to extract and determine trans, trans- muconic acid (tt-MA) from urine samples as a potential biomarker of low-level exposure to benzene. HPSs with controllable size and functional shells were synthesized through weak acid-base assembly under hydrothermal conditions. Hollow nanospheres can act as a storage reservoir or a nanoreactor, the functional shell not only provides a significant surface area for reactions, but also easily chelates target compounds through the abundant functional groups present in it. The main factors affecting the extraction performance, including sample volume, sample flow rate, elution volume, sample pH, type of washing solvent, and type of elution solvent, were evaluated and optimized through coupling to a high-performance liquid chromatography (HPLC-UV) analyzer. The highest recovery rate of tt-MA from urine with HPSs adsorbent was obtained at pH 7, sample volume 2 ml, sample flow rate 1 ml/min, deionized water/methanol (9,1 <em>v</em>/v) as washing solvent, and ethanol/acetic acid 3 % (8,2 v/v) as elution solvent. The optimized method was validated using three concentrations of 0.1, 25, and 50 μg/ml, and its within-day and day-to-day reproducibility was confirmed (RSD < 7.7 %). A good linear range (r <sup>2</sup> > 0.99) and low limits of detection (0.05 μg/ml) were obtained as well. The recovery of tt-MA from spiked urine samples in the quality control (QC) concentrations was more than 96 %, demonstrating the HPS-SPE method's applicability in the analysis of urine samples of benzene-exposed people.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124674"},"PeriodicalIF":2.8,"publicationDate":"2025-05-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144204666","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}

引用次数: 0

Development of a HILIC-MS/MS method for simultaneous quantification of lipophilic antitumor TriPPPro-prodrugs and their polar metabolites in HT29 cell extracts HT29细胞提取物中亲脂性抗肿瘤药物tripppro -前药物及其极性代谢物的HILIC-MS/MS同时定量方法的建立

IF 2.8 3区医学

Journal of Chromatography B Pub Date : 2025-05-28 DOI: 10.1016/j.jchromb.2025.124673

Michelle Vogts , Julian Witt , Maria Riedner , Chris Meier

{"title":"Development of a HILIC-MS/MS method for simultaneous quantification of lipophilic antitumor TriPPPro-prodrugs and their polar metabolites in HT29 cell extracts","authors":"Michelle Vogts , Julian Witt , Maria Riedner , Chris Meier","doi":"10.1016/j.jchromb.2025.124673","DOIUrl":"10.1016/j.jchromb.2025.124673","url":null,"abstract":"<div><div>Nucleoside analogues are among the most widely used antiviral and also antitumoral agents. The nucleoside analogues require intracellular metabolic activation through stepwise phosphorylation resulting in the bioactive nucleoside triphosphates. To directly deliver the active metabolite, our group developed a prodrug system where the nucleoside triphosphate (NTP) is masked by two lipophilic moieties which are enzymatically cleaved off after successful cellular uptake. To date, no data are available on the intracellular concentrations of the active metabolites responsible for the determined antiviral or antitumor activity.</div><div>In this paper, we describe the development of a HILIC-MS/MS method for the quantification of Tri<em>PPP</em>ro-prodrugs, derived from the anticancer drug fluorouracil (5-FU) and all resulting metabolites, FdU, FdU-monophosphate (MP), FdU-diphosphate (DP), and FdU-triphosphate (TP), in cancer cell lysate. Because of the different chemical properties of the lipophilic prodrugs and the hydrophilic metabolites, sample preparation as well as liquid chromatography method development were challenging factors. A liquid-liquid extraction protocol was employed and with use of hydrophilic liquid chromatography, the simultaneous retention of all analytes was guaranteed.</div><div>The method was validated for the following concentration ranges in cancer cell lysate and the associated supernatant: 2.0–1000 ng/mL.</div><div>The method was successfully applied to quantify prodrugs and metabolites in HT29 cancer cell lysate and supernatant samples after cellular uptake studies with two different Tri<em>PPP</em>ro-prodrugs. The method can also be employed for the quantification of other lipophilic prodrugs, as well as nucleotides and nucleosides (derivatives).</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124673"},"PeriodicalIF":2.8,"publicationDate":"2025-05-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144204665","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}

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