Journal of Chromatography B最新文献

{"title":"Application of preparative high-speed countercurrent chromatography for isolation of a bicyclo-[3.2.1]-octanoid neolignan from Piper multinodum C. DC. and determination of its absolute stereochemistry","authors":"André Mesquita Marques ,&nbsp;Lavínia de Carvalho Brito ,&nbsp;Ana Carolina Ferreira de Albuquerque ,&nbsp;Arthur Ribeiro de Souza ,&nbsp;Fernando Martins dos Santos Junior ,&nbsp;Adélia Viviane de Luna ,&nbsp;Maria Raquel Figueiredo ,&nbsp;Ygor Jessé Ramos ,&nbsp;Davyson de Lima Moreira","doi":"10.1016/j.jchromb.2025.124711","DOIUrl":"10.1016/j.jchromb.2025.124711","url":null,"abstract":"<div><div>This study aimed to propose a straightforward approach for isolating a novel neolignan compound using high-speed countercurrent chromatography (HSCCC) in combination with spectrometric techniques. The bicycleneolignan compound was detected in the dichloromethane partition obtained from methanolic leaf extract of <em>Piper multinodum</em>. After evaluating several two-phase solvent systems, the <em>n</em>-hexane/ethyl acetate/methanol/water in ratio 3:1:1:1 (<em>v</em>/v/<em>v</em>/v) demonstrated the highest efficiency for HSCCC separation of the target compound, as evidenced by the optimal distribution coefficient K_<em>D</em> value of 1.55, using the tail-to-head elution mode, yielding 87.0 mg in 96.7 %. Its relative structure and absolute stereochemistry were unequivocally determined through 1D and 2D-NMR spectroscopy and HRMS data, complemented by NMR quantum-mechanical calculations, and application of the DP4+ method, as well as electronic circular dichroism data. Our findings confirmed the identification of the new compound multinodine -(7<em>R</em>,8<em>S</em>,1′<em>R</em>,3′<em>R</em>) (E)7-(benzo[3,4]-dioxol-1-yl)-3′,6′-dimethoxy-8-methyl-1′-(prop-7′-en-7′-yl) bicyclo-[3.2.1]-oct-5′-en-4′-one).</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1264 ","pages":"Article 124711"},"PeriodicalIF":2.8,"publicationDate":"2025-06-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144562830","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":"Automated DBS-online SPE–LC–MS/MS platform with dynamic solvent dilution: Robust quantification of antipsychotic drugs for decentralized therapeutic drug monitoring","authors":"Yanxiao Zhou ,&nbsp;Huirong Li ,&nbsp;Mengjia Lin ,&nbsp;Jiwei Yang ,&nbsp;Xiaofeng Yu","doi":"10.1016/j.jchromb.2025.124704","DOIUrl":"10.1016/j.jchromb.2025.124704","url":null,"abstract":"<div><div>This study introduces a novel fully automated dried blood spot (DBS)-online solid-phase extraction (SPE)-LC-MS/MS system for the quantification of 19 antipsychotic drugs in dried blood spots, addressing critical challenges in therapeutic drug monitoring (TDM). By integrating dynamic online dilution technology, the system overcomes solvent incompatibility between DBS eluents (high organic content) and hydrophilic SPE sorbents, minimizing analyte loss during trapping. Moreover, the automated workflow eliminates manual intervention, achieving precision (CV ≤12 %), accuracy (RE ≤ ±10 %) and matrix-agnostic performance (ME%: −11.4 %–10.8 %, CV &lt;10 %). When validated across serum and whole blood matrices, the method demonstrated exceptional linearity (R² &gt; 0.99) and sensitivity (LOD: 0.01–0.71 ng/mL). Stability studies confirmed DBS integrity at extreme temperatures (40 °C to 2–8 °C), enabling cost-effective sample transport via standard postal services. Comparative analysis with offline LC–MS–MS revealed strong agreement, underscoring the method's equivalence to gold-standard techniques. The platform's automation, minimal matrix dependency, and robustness position it as a transformative solution for decentralized TDM, particularly in resource-limited settings</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124704"},"PeriodicalIF":2.8,"publicationDate":"2025-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144365933","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":"Improved column chromatography–thin layer chromatography densitometry method for purification of dairy sphingomyelin","authors":"Jun Cai ,&nbsp;Yu Liu ,&nbsp;Chaoting Wen ,&nbsp;Xiaofang Liu ,&nbsp;Jixian Zhang ,&nbsp;Youdong Li ,&nbsp;Guoyan Liu ,&nbsp;Xin Xu ,&nbsp;Li Liang","doi":"10.1016/j.jchromb.2025.124708","DOIUrl":"10.1016/j.jchromb.2025.124708","url":null,"abstract":"<div><div>Sphingomyelin (SM) has the potential to be widely used in the food, cosmetics and pharmaceutical industries. However, SM is found in trace amounts in substances such as egg yolk and dairy products. Traditional purification methods, such as solvent extraction and column chromatography, have several drawbacks, including low purity, high loss and high solvent consumption, as well as complicated operation. These factors make efficiently separating high-purity SM difficult. In this work, a gradient elution silica gel column chromatography method dynamically monitored by TLC was developed for the purification of SM from milk phospholipid (MPL). First, the TLC elution conditions were optimized as follows: solvent methyl acetate–isopropanol–chloroform–methanol-0.25 % (w/v) potassium chloride (25:25:25:10:9, v/v/v/v/v/v), spot volume of 50–75 μg MPL or 5–7.5 μg SM sample, separation distance of 16 cm and 25 °C. Then, the relative quantification of SM was performed in combination with ImageJ software, and the method was confirmed to be accurate and reliable through a comprehensive evaluation of its precision, accuracy, LOD and LOQ. Finally, the optimized silica gel column chromatography method was used for the purification of SM by TLC dynamic monitoring, and the methyl acetate–isopropanol–dichloromethane–methanol–water system (25:25:25:10:11, v/v/v/v/v) was used as the first eluent, and the dichloromethane–methanol–water system (45:30:8.5, v/v/v) was used as the second eluent. SM recoveries exceeded 85 % under the optimal conditions of silica gel sample volumes of 3.125–3.75 mg/g and a diameter-to-height ratio of 1:5–1:6. The purity of SM prepared by the above method reached 90 % (molar ratio) as determined by ³¹P NMR, and SM had a higher percentage of esterified long chain saturated fatty acids (more than 20 carbon atoms) as determined by UPLC-MS/MS.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124708"},"PeriodicalIF":2.8,"publicationDate":"2025-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144322005","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":"In-syringe polypropylene fiber-supported liquid microextraction using natural deep eutectic solvents for the convenient analysis of amphetamine-type stimulants in biological and environmental samples","authors":"Yabing Shan ,&nbsp;Jiayi Li ,&nbsp;Ying Chen ,&nbsp;Rui Jia ,&nbsp;Xianbin Zeng ,&nbsp;Yingying Li ,&nbsp;Di Chen ,&nbsp;Dongmei Li","doi":"10.1016/j.jchromb.2025.124701","DOIUrl":"10.1016/j.jchromb.2025.124701","url":null,"abstract":"<div><div>This study introduces an environmentally friendly and efficient sample preparation method for the extraction and analysis of amphetamine-type stimulants (ATS) in biological and environmental samples. The proposed polypropylene fiber-supported liquid-phase microextraction (PPF-SLME) method utilizes PPF as the support medium and natural deep eutectic solvents (NADES) as the extractant, coupled with a simple in-syringe format for streamlined extraction and desorption processes. The use of pure PPF, sourced from disposable three-layer nonwoven face masks, offers a cost-effective and sustainable alternative to conventional natural fibers. Additionally, NADES, composed of natural and environmentally benign components, enhances the overall sustainability of the method. This approach reduces solvent consumption while improving extraction efficiency, making it a green alternative to traditional methods. The optimized extraction conditions—including NADES composition, solvent volumes, and the number of pull-push cycles—were systematically evaluated. The method exhibited robust linearity within the concentration range of 0.01–10 ng/mL, featuring an R² value greater than 0.994, and detection limits spanning from 1 to 6 ng/L. Relative recoveries ranged from 81.8% to 104.8%, with relative standard deviations below 10.6%. The method's performance was successfully demonstrated in both environmental and biological sample analyses, providing a rapid, cost-effective, sensitive, and sustainable solution for ATS detection.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124701"},"PeriodicalIF":2.8,"publicationDate":"2025-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144365934","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":"In vivo sequential metabolism by UPLC/MS, network pharmacology and cell experimentation for screening Q-markers of Penthorum chinense Pursh","authors":"Miao Hou ,&nbsp;Ying Chen ,&nbsp;Yue Jiang ,&nbsp;Xinyi Zhu ,&nbsp;Huimin Zhang ,&nbsp;Tianqin Xiong ,&nbsp;Zhipeng Deng","doi":"10.1016/j.jchromb.2025.124709","DOIUrl":"10.1016/j.jchromb.2025.124709","url":null,"abstract":"<div><div>PCP (<em>Penthorum chinense</em> Pursh) is a traditional Chinese medicine of Miao nationality, and is used to prevent and treat liver diseases. Modern research shows that it has anti-hepatitis virus, anti-hepatic fibrosis and anti-oxidation effects. It has certain curative effect on cholestatic liver injury (CLI). However, the quality marker (Q-marker) of PCP in the treatment of CLI is still unclear. This study aims to explore and screen the Q-markers of PCP using a novel multi-dimensional strategy of <em>in vivo</em> sequential metabolism, network pharmacology and cell experimentation. Sequential metabolism in rats identified 18 prototypes and 123 metabolites, primarily flavonoids, with hydroxylation, reduction, acetylation, and glucuronidation as the main metabolic pathways. A total of 23 inherent components of PCP were identified, including 18 prototype components exposed in blood and 5 prototypes inferred from reverse tracing of their metabolites. Network pharmacology analysis revealed six potential Q-markers for the treatment of CLI: pinocembrin, apigenin, alpinetin, naringenin, pinocembrin-7-O-β-D-glucoside, and 5-methoxy pinocembroside. The core therapeutic targets were identified as TNF, AKT1, and ESR1. Molecular docking analysis demonstrated that all the six potential Q-markers exhibited binding energies below −6.5 kcal/mol with targets, suggesting their significant role in CLI treatment. Cell experiments indicated that six Q-markers had certain pharmacological activity against CLI. Furthermore, quantification of six Q-markers demonstrated that their content remained relatively stable across 12 batches of Gansu Granules. These findings provide a material basis for the quality control and development of PCP.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 124709"},"PeriodicalIF":2.8,"publicationDate":"2025-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144330756","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":"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 ,&nbsp;Rahman Emamzadeh ,&nbsp;Nastaran Masoudi-Khorram ,&nbsp;Mahboobeh Nazari ,&nbsp;Fereshteh Abdolmaleki ,&nbsp;Mohammad Kangarani-Farahani","doi":"10.1016/j.jchromb.2025.124697","DOIUrl":"10.1016/j.jchromb.2025.124697","url":null,"abstract":"","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1263 ","pages":"Article 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}