Journal of Chromatography B最新文献

{"title":"Facile and green synthesis of PFP@SiO2 as stationary phase for liquid chromatography and its application for pharmaceutical analysis","authors":"Xuerui Zhang ,&nbsp;Shuo Wang ,&nbsp;Yixin Ren ,&nbsp;Xiaoting Fu ,&nbsp;Xiaodong Bi ,&nbsp;Xia Wang ,&nbsp;Ru-Song Zhao","doi":"10.1016/j.jchromb.2025.124706","DOIUrl":"10.1016/j.jchromb.2025.124706","url":null,"abstract":"<div><div>The pentafluorophenyl (PFP)-functionalized stationary phases, due to their unique hydrophobicity and fluorophilic affinity, have received increasing attention in separation science. How to introduce PFP group effectively with a green chemistry approach has become an important issue. This work provided a facile and green synthetic route for preparing PFP@SiO₂ column. The liquid chromatography (LC) performance towards pharmaceutical molecules such as phenolic acids, flavonoids, and antiviral drugs was systematically explored. The results showed the PFP@SiO₂ column possessed a low back pressure and good solvent endurance (less affected by solvent effect). Under gradient elution mode, the column also showed a higher separation efficiency and good quantitative capacity towards complex natural product (<em>Sanguisorbae Radix Carbonisatum</em> extract), which met the requirements of current standards and regulations. This work provides a facile green synthesis approach for preparing highly-performed PFP@SiO₂ column for pharmaceutical applications, and a powerful tool for biomedicine.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124706"},"PeriodicalIF":2.8,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144307803","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":"Chemical analysis-relating nomenclature issues in the Journal of Chromatography B","authors":"David S. Hage,&nbsp;Huwei Liu,&nbsp;Georgios Theodoridis,&nbsp;Dimitrios Tsikas,&nbsp;Christina Virgilliou,&nbsp;Ian Wilson","doi":"10.1016/j.jchromb.2025.124703","DOIUrl":"10.1016/j.jchromb.2025.124703","url":null,"abstract":"","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124703"},"PeriodicalIF":2.8,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144312621","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":"Refining proteoform characterization in biopharmaceuticals: A paradigm for the impact of pI markers and carrier ampholytes in imaged capillary isoelectric focusing tandem mass spectrometry","authors":"Teresa Kwok,&nbsp;She Lin Chan,&nbsp;Niusheng Xu,&nbsp;Tiemin Huang,&nbsp;Tao Bo","doi":"10.1016/j.jchromb.2025.124705","DOIUrl":"10.1016/j.jchromb.2025.124705","url":null,"abstract":"<div><div>Proteoforms, structurally distinct yet closely related protein isoforms, play a pivotal role in biopharmaceutical development, directly influencing therapeutic efficacy, safety, and stability. These molecular variants arise from genetic polymorphisms, alternative splicing, and post-translational modifications, necessitating advanced analytical techniques for precise characterization. Imaged capillary isoelectric focusing (icIEF) coupled with mass spectrometry (MS) has become a powerful high-resolution tool for resolving and identifying proteoforms in complex biopharmaceutical samples. This study used a monoclonal antibody (mAb) as a paradigm to comprehensively evaluate the chemical properties of pI markers and carrier ampholytes in icIEF-MS. By investigating their effects on method accuracy, sensitivity, MS compatibility, and repeatability, we demonstrated how reagent selection can impact overall assay performance. The MS characterization of these reagents provided deeper insights into their influence on icIEF separation and proteoform identification, offering a critical case study for optimizing diverse icIEF reagent strategies. These findings contribute to the advancement of icIEF-MS methodologies, ensuring robust and reproducible proteoform characterization for biopharmaceutical research, process development, and quality control.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124705"},"PeriodicalIF":2.8,"publicationDate":"2025-06-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144290582","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":"Quantitative determination of Selinexor concentrations in plasma samples from children with non-rhabdomyosarcoma soft-tissue sarcomas: Troubleshooting plasma instability issues","authors":"Sreenath Nair ,&nbsp;Thandranese Owens ,&nbsp;Abigail Stolarski ,&nbsp;Jessica Gartrell ,&nbsp;Christopher Tinkle ,&nbsp;Clinton F. Stewart","doi":"10.1016/j.jchromb.2025.124700","DOIUrl":"10.1016/j.jchromb.2025.124700","url":null,"abstract":"<div><div>Selinexor (KPT-330), a first-in-class, CNS-penetrant oral inhibitor of Exportin-1, disrupts the nuclear export of tumor suppressor proteins, promoting their accumulation and inducing cancer cell death. In this study, a reliable and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and validated to quantify selinexor concentrations in human plasma. A standard solid-phase extraction method using an Oasis HLB μElution plate was utilized to isolate selinexor and its internal standard, selinexor-d₃, from human plasma. The chromatographic separation was executed on a reversed-phase analytical column with a binary gradient of water and acetonitrile, both containing 0.1 % formic acid, at a flow rate of 0.5 mL/min. Mass spectrometry detection was performed in positive ion mode by tracking the mass transitions of 444.0 &gt; 334.0 for selinexor and 447.0 &gt; 333.9 for selinexor-d₃. The developed LC-MS/MS assay for selinexor was rigorously validated over a wide range of clinically relevant concentrations (1–1000 ng/mL, r² ≥ 0.99) in accordance with FDA bioanalytical method validation guidelines. The method exhibited inter-day accuracy, expressed as relative error (R.E.), ranging from 2.28 % to 4.38 %, with precision values not exceeding 5.92 %. Intra-day accuracy showed R.E. values between 0.24 % and 7.30 %, accompanied by precision values ≤4.81 %. Additionally, the method demonstrated high extraction recovery, ranging from 82.80 % to 87.87 %, and a negligible matrix effect. The pH adjustments applied to the plasma prior to storage and processing maintained the stability of selinexor under several experimental conditions, including multiple freeze-thaw cycles and long-term storage at −80 °C. As proof of principle, the LC-MS/MS assay was successfully applied to a phase I clinical pharmacokinetic study of selinexor in pediatric patients with non-rhabdomyosarcoma soft tissue sarcomas, yielding reliable and reproducible measurements of selinexor concentrations in plasma.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124700"},"PeriodicalIF":2.8,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144297058","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":"Corrigendum to \"Immobilization of albumin binding domain (ABD) on Sepharose 4B and magnetic particle for efficient single-step purification of human serum albumin\" [J. Chromatogr. B 1261 (2025) 124655].","authors":"Maryam Nazari, Rahman Emamzadeh, Nastaran Masoudi-Khorram, Mahboobeh Nazari, Fereshteh Abdolmaleki, Mohammad Kangarani-Farahani","doi":"10.1016/j.jchromb.2025.124697","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124697","url":null,"abstract":"","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":" ","pages":"124697"},"PeriodicalIF":2.8,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144281920","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":"LC-MS/MS analysis of five antibiotics in dried blood spots for therapeutic drug monitoring of ICU patients","authors":"Zhan Qi,&nbsp;Sha Zhang,&nbsp;Jie Li,&nbsp;Shijing Qian,&nbsp;Danfei Song,&nbsp;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> &gt; 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}

{"title":"Absolute quantitative lipidomics of Clonorchis sinensis-infected rats reveals key alterations in metabolic pathways","authors":"Zhenli Xu ,&nbsp;Shiwen Hua ,&nbsp;Jian Ding ,&nbsp;Xinyi Hu ,&nbsp;Rui Chen ,&nbsp;Yang Cheng ,&nbsp;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}

{"title":"Quantification of amikacin, gentamicin, and tobramycin in capillary plasma microsamples by LC-MS/MS","authors":"Ana Paula Grando ,&nbsp;Ana Carolina Fritsch ,&nbsp;Amanda Pacheco Bondan ,&nbsp;Carolina Weber Ferrareze ,&nbsp;Giovana Piva Peteffi ,&nbsp;Roberta Zilles Hahn ,&nbsp;Ana Júlia Dossena ,&nbsp;Juliana Raquel Raasch ,&nbsp;Marina Venzon Antunes ,&nbsp;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⁺® 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> &lt; 0.0001) and GEN (<em>r</em> = 0.979, <em>P</em> &lt; 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}

{"title":"Xuefu Zhuyu decoction ameliorates atherosclerosis in ApoE−/− mice by regulating cholesterol metabolism and inflammation","authors":"Yaobin Zhu ,&nbsp;Yonghao Chen ,&nbsp;Ruxi Tong ,&nbsp;Xuanbin Huang ,&nbsp;Bilin Xu ,&nbsp;Jinshui Chen ,&nbsp;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^−/− mice fed with a high-fat diet, as well as the latent molecular mechanisms involved.</div></div><div><h3>Methods</h3><div>ApoE^−/− 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}

{"title":"Simulation of sildenafil metabolism using an electrochemical oxidation system","authors":"Unyong Kim ,&nbsp;Sumin Seo ,&nbsp;Jiyu Kim ,&nbsp;Chohee Jeong ,&nbsp;Woojin Jeong ,&nbsp;Han Young Eom ,&nbsp;Joon Hyuk Suh ,&nbsp;Junghyun Kim ,&nbsp;Hyun-Deok Cho ,&nbsp;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}