Biomedical Chromatography最新文献_第6页

Resolution and Quantitation of Ribonucleosides and Deoxyribonucleosides in Digested Genomic DNA by UHPLC–MS/MS UHPLC-MS /MS法测定基因组DNA中核糖核苷和脱氧核糖核苷的含量

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-13 DOI: 10.1002/bmc.70599

Joshua J. Deppas, Reyna Jones, Robert A. Parise, Pinakin Pandya, Christopher J. Bakkenist, Jan H. Beumer

{"title":"Resolution and Quantitation of Ribonucleosides and Deoxyribonucleosides in Digested Genomic DNA by UHPLC–MS/MS","authors":"Joshua J. Deppas, Reyna Jones, Robert A. Parise, Pinakin Pandya, Christopher J. Bakkenist, Jan H. Beumer","doi":"10.1002/bmc.70599","DOIUrl":"https://doi.org/10.1002/bmc.70599","url":null,"abstract":"Deoxyuridine (dUrd) is often misincorporated into genomic DNA in cancer patients receiving antimetabolite chemotherapy. This activates base excision repair and recruits ataxia telangiectasia-mutated and Rad3-related (ATR), which coordinates DNA repair with nucleotide metabolism by facilitating ribonucleotide reductase (RNR) activity. Ceralasertib (AZD6738) is the most clinically advanced ATR inhibitor (ATRi) and may abrogate this regulatory pathway and diminish RNR-mediated deoxynucleotide triphosphate synthesis. To further understand ATRi-induced dUrd misincorporation, we developed a highly sensitive LC–MS/MS method to quantitate: deoxyuridine, uridine, guanosine, adenosine, cytidine, thymidine, deoxyguanosine, deoxyadenosine, and deoxycytidine from digested genomic DNA.Assay application was demonstrated with genomic DNA digested from multiple murine cell lines treated with ceralasertib. Chromatographic separation was achieved with an Inertsil ODS-3 (150 × 2.1 mm, 3 μm) column and a gradient elution program of 0.1% formic acid in water and 0.1% formic acid in methanol over an 18-min run time. Detection was performed on a SCIEX 6500+ tandem mass spectrometer. The method proved to be accurate (90.8%–114.2%) and precise (< 7.73% CV) across analytes. Freeze–thaw stability (106.4%–114.3%), stability for 12 months at −80°C (88.7%–113.7%), and stability for 4 h at room temperature (104.1%–114.0%) were acceptable across QCs.","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/bmc.70599","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148719191","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Principle-Guided Multistep Workflow for Screening Potential Quality Marker Candidates of Sanqi Shangyao Tablet Based on UHPLC-Q-Orbitrap MS, In Silico Screening, and In Vitro Validation. 基于UHPLC-Q-Orbitrap质谱、硅筛选和体外验证的三七上药片潜在质量标记物筛选多步骤流程

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-01 DOI: 10.1002/bmc.70554

Ban Chen, Huiyin Xia, Yanxiu Li, Jun Ji, Yuchen Hu, Hongwei Song, Yingqing Zhang, Xican Li

{"title":"A Principle-Guided Multistep Workflow for Screening Potential Quality Marker Candidates of Sanqi Shangyao Tablet Based on UHPLC-Q-Orbitrap MS, In Silico Screening, and In Vitro Validation.","authors":"Ban Chen, Huiyin Xia, Yanxiu Li, Jun Ji, Yuchen Hu, Hongwei Song, Yingqing Zhang, Xican Li","doi":"10.1002/bmc.70554","DOIUrl":"10.1002/bmc.70554","url":null,"abstract":"Quality marker (Q-marker) screening is crucial for the quality control of traditional Chinese medicine (TCM) formulas but remains challenging. In this study, a principle-guided multistep strategy was established for the rational identification of potential Q-marker candidates in Sanqi Shangyao tablet (SST). Ultrahigh-performance liquid chromatography coupled with quadrupole-Orbitrap mass spectrometry was employed for comprehensive chemical profiling, followed by traceability assessment and relative specificity estimation. A total of 124 compounds were characterized, among which 66 were confirmed using authentic standards. After successive filtering based on traceability, relative specificity, and drug-like properties, 25 candidate compounds were retained and associated with 163 osteoarthritis-related targets. Enrichment analysis identified the TNF signaling pathway as a key regulatory axis, and network topology analysis prioritized prunetin for further investigation. In IL-1β-stimulated chondrocytes, prunetin showed no apparent cytotoxicity at concentrations up to 50 μM, significantly reduced nitric oxide production, suppressed pro-inflammatory mediators, and attenuated extracellular matrix degradation. Molecular dynamics simulations provided supportive structural evidence for favorable interactions between prunetin and representative targets, including MAPK14, PTGS2, and AKT1. Based on integrated chemical, biological, and TCM theory considerations, six compounds were proposed as potential Q-marker candidates. This study provides a practical workflow for preliminary Q-marker candidate prioritization in complex herbal formulations.","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 8","pages":"e70554"},"PeriodicalIF":1.7,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13370256/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148444161","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Simple and Sensitive LC-MS/MS Method for Simultaneous Quantification of Dasatinib and Erythromycin in Mice Plasma: Application to Preclinical Pharmacokinetic Study. 同时测定小鼠血浆中达沙替尼和红霉素含量的LC-MS/MS方法在临床前药代动力学研究中的应用

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-01 DOI: 10.1002/bmc.70533

Avinash Kumar, Nirbhay Kumar Tiwari, Sanjeev Giri, Ramesh Patnam, Rameshwar Ameta

{"title":"A Simple and Sensitive LC-MS/MS Method for Simultaneous Quantification of Dasatinib and Erythromycin in Mice Plasma: Application to Preclinical Pharmacokinetic Study.","authors":"Avinash Kumar, Nirbhay Kumar Tiwari, Sanjeev Giri, Ramesh Patnam, Rameshwar Ameta","doi":"10.1002/bmc.70533","DOIUrl":"10.1002/bmc.70533","url":null,"abstract":"Dasatinib (DAS) is a tyrosine kinase inhibitor used in the treatment of chronic myeloid leukemia (CML) and erythromycin (ERY) is macrolide antibiotic used to treat a range of inflammatory conditions are often co-administered in clinical practice. The simultaneous estimation of DAS and ERY helps in understanding the pharmacokinetics and drug-drug interactions. In this respect, we presented novel, sensitive, and validated bio-analytical LC-ESI-MS/MS method for simultaneous estimation of DAS and ERY in CD-1 mice plasma. The LLOQ was 2.0 ng/mL with an S/N ratio of 15. This validated method was used to study the PK of DAS and ERY in mice following intravenous and oral administration. The DAS was administered at 5 mg/kg via both oral and intraveneous route, whereas ERY was administered at 50 mg/kg orally and 5 mg/kg intraveneousaly. Following intravenous dosing, DAS showed high clearance and distribution, while ERY exhibited high clearance and distribution. The oral bioavailability was 64% for DAS and 21% for ERY. When co-administered orally at 5 mg/kg for DAS and 50 mg/kg of ERY, the AUC and Cmax of DAS were unchanged. However, the systemic exposure (w.r.t AUC and Cmax) of ERY was slightly higher (2.4-fold) in the presence of DAS, which may be attributed because of the CYP3A4 inhibition potential.","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 8","pages":"e70533"},"PeriodicalIF":1.7,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13353865/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148418303","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Overcoming Stability Challenge During the Quantification of SHR6508 in Human Plasma by LC-MS/MS. LC-MS/MS法测定人血浆中SHR6508的稳定性挑战

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-01 DOI: 10.1002/bmc.70555

Yuan Wu, Tao Chen, Kan Zhong, Laiyou Wang

{"title":"Overcoming Stability Challenge During the Quantification of SHR6508 in Human Plasma by LC-MS/MS.","authors":"Yuan Wu, Tao Chen, Kan Zhong, Laiyou Wang","doi":"10.1002/bmc.70555","DOIUrl":"10.1002/bmc.70555","url":null,"abstract":"SHR6508, a novel calcimimetic agent, is currently being developed for treating secondary hyperparathyroidism in chronic kidney disease (CKD) patients requiring maintenance hemodialysis. For the purpose of quantifying SHR6508 in human plasma, a sensitive and reliable LC-MS/MS method was first developed and successfully validated. Since SHR6508 is a disulfide bond-containing peptide, ascorbic acid was supplemented into blood samples during collection to prevent thiol-disulfide exchange reactions. Plasma matrix samples were processed by protein precipitation with a water-acetonitrile solution (1:4, v/v) containing 0.05% formic acid. Chromatographic separation was conducted on an XBridge Peptide BEH C18 column (4.6 × 100 mm, 5.0 μm) under gradient elution with water and methanol, each containing 0.1% trifluoroacetic acid. SHR6508 was quantified by tandem mass spectrometry in positive electrospray ionization using multiple reaction monitoring with transitions of m/z 532.0 → 455.5 for SHR6508 and m/z 537.0 → 456.5 for SHR180296 (isotope-labelled internal standard). The quantification linear range was 1.00-1000 ng/mL. All validation parameters including selectivity, carryover, precision, accuracy, recovery, and matrix effect fell within the predefined acceptance criteria. The stabilization strategy developed in this work may also offer valuable insights for the collection and analysis of other disulfide bond-containing peptide drugs.","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 8","pages":"e70555"},"PeriodicalIF":1.7,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13355117/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148418300","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Development and Validation of a Sensitive UHPLC-MS/MS Analytical Method for Fulzerasib in Rat Plasma and its Application to Pharmacokinetics Studies. 大鼠血浆中富泽拉西布的高效液相色谱-质谱联用分析方法的建立与验证及其在药代动力学研究中的应用。

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-01 DOI: 10.1002/bmc.70552

Qiang Liu, Jin-Zhu Zhao, Li Wang, Fu-Sheng Zhou, Jiong Lan, Qiang Lu, Tao Jiang, Hong-Can Ren

{"title":"Development and Validation of a Sensitive UHPLC-MS/MS Analytical Method for Fulzerasib in Rat Plasma and its Application to Pharmacokinetics Studies.","authors":"Qiang Liu, Jin-Zhu Zhao, Li Wang, Fu-Sheng Zhou, Jiong Lan, Qiang Lu, Tao Jiang, Hong-Can Ren","doi":"10.1002/bmc.70552","DOIUrl":"10.1002/bmc.70552","url":null,"abstract":"Fulzerasib is a novel, potent, and irreversible covalent inhibitor targeting the KRAS G12C mutation, recently approved in China for advanced nonsmall cell lung cancer. This study aimed to develop and fully validate a rapid, specific and sensitive UHPLC-MS/MS method for the quantification of Fulzerasib in rat plasma. Sample preparation was streamlined using a simple protein precipitation technique with acetonitrile. Chromatographic separation was achieved within a 4.0-min run on a C18 column, with verapamil as the internal standard and detection via multiple reaction monitoring. The method was rigorously validated over a linear range of 5 to 5000 ng/mL (R2 > 0.9933), demonstrating excellent accuracy (102%-112.7%) and precision (≤ 10.3% for QCs). Stability was confirmed under various storage and processing conditions. The validated method was successfully applied in the first pharmacokinetic study of Fulzerasib in Sprague-Dawley rats following single intravenous (1 mg/kg) and oral (3 mg/kg) administration. Fulzerasib exhibited favorable pharmacokinetic properties, including low plasma clearance (5.02 mL/min/kg), moderate volume of distribution and notably high oral bioavailability of 38.6%. The established method is reliable, efficient and readily applicable, thereby providing a vital tool for accelerating the ongoing preclinical and translational research of Fulzerasib.","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 8","pages":"e70552"},"PeriodicalIF":1.7,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13369354/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148444242","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Preparation of Silica-Based Chitosan Chiral Stationary Phases by Two Synthetic Approaches and Evaluation of Their Enantioseparation Performance by HPLC. 两种合成方法制备硅基壳聚糖手性固定相及其对映体分离性能的HPLC评价。

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-01 DOI: 10.1002/bmc.70546

Xingjing Zhang, Baohe Li, Xiaoqian Han

{"title":"Preparation of Silica-Based Chitosan Chiral Stationary Phases by Two Synthetic Approaches and Evaluation of Their Enantioseparation Performance by HPLC.","authors":"Xingjing Zhang, Baohe Li, Xiaoqian Han","doi":"10.1002/bmc.70546","DOIUrl":"10.1002/bmc.70546","url":null,"abstract":"Chitosan derivatives play an important role in chiral separation due to their excellent chiral recognition properties. However, the preparation of chitosan derivatives with good chiral separation performance and resistance to organic solvents still needs to be explored. Here, we prepared the chitosan (4-chlorophenylaminoformate) derivatives as the corresponding chiral stationary phases CSP-1 and CSP-2 through coating and bonding methods and compared them with CSP-3 prepared by changing the position of the chlorine substitution on the phenyl group. This revealed the interaction between the chitosan-type chiral selectors (CSs) and the chiral analytes during the chiral separation process. The enantioseparation capability of the CSPs was evaluated using high-performance liquid chromatography (HPLC). The CSPs demonstrated good enantioseparation performance for most of the tested chiral analytes, and the enantioselective separation of flucloxacillin was comparable with that of commercial Chiralcel OD-H and Chiralpak AD-H. We gained a deeper understanding of the chiral recognition mechanism by modifying the mobile phase composition and the position of chlorine substituents in the phenyl group. Furthermore, the CSP-2 overcomes the dissolution and high expansion problems of traditional coating-type CSP in unconventional eluents, and the separation performance achieved for some of the tested chiral compounds is even superior to that of CSP-1.","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 8","pages":"e70546"},"PeriodicalIF":1.7,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13373977/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148468661","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Development of Liquid-Liquid Extraction-Assisted, Derivatization-Free Gas Chromatography Integrated With the Flame Ionization Detection (GC-FID) Method for the Direct Determination of Fatty Acids in Cream Formulations. 液-液萃取辅助、无衍生化气相色谱-火焰离子化检测（GC-FID）直接测定乳膏制剂中脂肪酸的方法的建立。

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-01 DOI: 10.1002/bmc.70548

Ruchi Bhatia, Deepti Jain

{"title":"Development of Liquid-Liquid Extraction-Assisted, Derivatization-Free Gas Chromatography Integrated With the Flame Ionization Detection (GC-FID) Method for the Direct Determination of Fatty Acids in Cream Formulations.","authors":"Ruchi Bhatia, Deepti Jain","doi":"10.1002/bmc.70548","DOIUrl":"10.1002/bmc.70548","url":null,"abstract":"Marketed cream formulations contain fatty acids as core constituents, required for its texture, uniformity, shelf life, and skin penetration. Given their importance in the cosmetic and pharmaceutical industries, real-time quantification and analysis of these compounds are crucial for assessing authenticity and ensuring compliance with regulatory specifications. In the present analysis, we employed gas chromatography with flame ionization detection (GC-FID) due to its sensitivity, robustness, and quantitative reliability. Overcoming the traditional method for fatty acid determination, we analyzed the sample without derivatization to fatty acid methyl esters (FAMEs). The derivatization step was initially omitted to simplify sample preparation, reduce analysis time and reagent consumption, and minimize the potential errors associated with incomplete esterification or degradation of unstable fatty acids during derivatization. Direct analysis was performed by dissolving the extracted sample in isopropyl alcohol and then filtering and injecting it into the GC-FID system under optimized chromatographic conditions. The optimized method was used for the concurrent quantification of lauric, myristic, palmitic, oleic, and stearic acids. The validation of the present work was executed in alignment with ICH Q2(R1) requirements. The method was further expanded to analyze real cream samples, thereby validating the accuracy of fatty acid profiling for routine quality control.","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 8","pages":"e70548"},"PeriodicalIF":1.7,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13367021/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148434713","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Development and Validation of a UPLC-MS/MS for Determination of Loureirin D in Rat Plasma and Its Application to Pharmacokinetics. UPLC-MS/MS法测定大鼠血浆中洛瑞素D及其药代动力学研究

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-01 DOI: 10.1002/bmc.70547

Yi Zhou, Yuxin Wu, Chenyao Xu, Chenbin Zhang, Congcong Wen, Xianqin Wang, Jianbo Li

{"title":"Development and Validation of a UPLC-MS/MS for Determination of Loureirin D in Rat Plasma and Its Application to Pharmacokinetics.","authors":"Yi Zhou, Yuxin Wu, Chenyao Xu, Chenbin Zhang, Congcong Wen, Xianqin Wang, Jianbo Li","doi":"10.1002/bmc.70547","DOIUrl":"10.1002/bmc.70547","url":null,"abstract":"Loureirin D is a bioactive dihydrochalcone isolated from Dracaena resin with very high therapeutic value. A sensitive and high-throughput ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS) method was developed for the quantitative analysis of loureirin D in rat plasma with only 50 μL of sample per assay. Sample extraction was protein precipitation using acetonitrile, and isoscoparin was used as internal standard (IS). Separation was achieved on the BEH C18 column with a gradient mobile phase of 0.1% (v/v) aqueous formic acid and acetonitrile. Detection was achieved with negative-ion electrospray ionization (ESI) detector in the multiple reaction monitoring (MRM) mode. The method was validated and proved to be linear in the concentration range of 2-2400 ng/mL (r ≥ 0.995), intraday and interday precision (RSD) was < 15%, and accuracy was 93.3%-110.1%. The extraction recovery was 88.7%-94.4%, and the matrix effects were 87.3%-92.9%. UPLC-MS/MS was used in pharmacokinetics in the rats after administration of loureirin D. The AUC(0-t) after intravenous administration (1 mg/kg) was 2074.7 ± 180.3 ng · h/mL, and AUC(0-t) after oral administration (5 mg/kg) was 563.4 ± 61.4 ng · h/mL; the absolute oral bioavailability was 5.4%. Pharmacokinetics showed rapid absorption, large Vz/F (52.7 ± 10.7 L/kg), high CLz/F (8.8 ± 0.9 L/h/kg), and extensive first-pass metabolism.","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 8","pages":"e70547"},"PeriodicalIF":1.7,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13355102/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148418338","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Critical Comparative Review of Analytical Techniques for Cloxacillin and Oxacillin Across Diverse Matrices Cloxacillin和Oxacillin跨不同基质分析技术的关键比较综述。

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-07-28 DOI: 10.1002/bmc.70571

Hemn A. H. Barzani, Rebaz Anwar Omer, Khalamala Ibrahim Salih Barzani, Hunar Yasin Muhammad, Ali Sedeeq Noaman, Kovan Dilawer Issa, Seerwan Hamadameen Sulaiman

{"title":"A Critical Comparative Review of Analytical Techniques for Cloxacillin and Oxacillin Across Diverse Matrices","authors":"Hemn A. H. Barzani, Rebaz Anwar Omer, Khalamala Ibrahim Salih Barzani, Hunar Yasin Muhammad, Ali Sedeeq Noaman, Kovan Dilawer Issa, Seerwan Hamadameen Sulaiman","doi":"10.1002/bmc.70571","DOIUrl":"10.1002/bmc.70571","url":null,"abstract":"<div>\u0000 \u0000 Cloxacillin (CLX) and oxacillin (OXA), two isoxazolyl β-lactam antibiotics widely used against penicillinase-producing Staphylococcus aureus, have attracted increasing attention due to their environmental persistence, residue occurrence, and analytical complexity across diverse matrices. This review provides a critical and integrated comparison of analytical techniques for the determination of CLX and OXA in pharmaceutical, biological, food, and environmental samples, addressing key challenges, including β-lactam instability, low intrinsic detectability, strong protein binding, and matrix interferences. Chromatographic methods, particularly HPLC and LC–MS/MS, remain the most reliable approaches, offering high selectivity and stability-indicating capability, with LC–MS/MS achieving superior sensitivity at ng/mL levels suitable for trace analysis, albeit at higher cost and with greater operational demands. Electrochemical techniques, especially nanomaterial- and molecularly imprinted-based sensors, demonstrate promising sensitivity and rapid response, though limitations in reproducibility and standardization persist. In contrast, spectroscopic methods are economical and simple but restricted by low sensitivity and poor selectivity in complex matrices. Overall, no single technique is universally optimal, and analytical performance is strongly matrix-dependent. Future perspectives should prioritize the development of hybrid, standardized, and green analytical platforms that balance sensitivity, robustness, and cost-effectiveness, alongside harmonized validation strategies to enable reliable and sustainable monitoring of CLX and OXA in real-world applications.\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 9","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-07-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148598498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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

Simultaneous Estimation of Avutometinib and Defactinib in Rat Plasma by Using LC–MS/MS and Its Application to Pharmacokinetic Studies LC-MS/MS同时测定大鼠血浆中阿乌托替尼和去法替尼的含量及其在药动学研究中的应用

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-07-28 DOI: 10.1002/bmc.70580

Kunduru Praveen, Sibbala Subramanyam, Jithendra Chimakurthy

{"title":"Simultaneous Estimation of Avutometinib and Defactinib in Rat Plasma by Using LC–MS/MS and Its Application to Pharmacokinetic Studies","authors":"Kunduru Praveen, Sibbala Subramanyam, Jithendra Chimakurthy","doi":"10.1002/bmc.70580","DOIUrl":"10.1002/bmc.70580","url":null,"abstract":"<div>\u0000 \u0000 The combination of avutometinib, a dual RAF/MEK inhibitor targeting the MAPK pathway, and defactinib, a selective focal adhesion kinase (FAK) inhibitor, represents a recently approved combination therapy for patients with KRAS-mutated or KRIS-mutated recurrent LGSOC (low-grade serous ovarian cancers). A comprehensive review of the literature indicates that although clinical studies have demonstrated the therapeutic potential of this combination, limited information is available regarding simultaneous quantification in biological matrices. Therefore, the present study mainly focused on a rapid selective and specific LC–MS/MS method that was developed and fully validated for the estimation of avutometinib and defactinib in rat plasma. Chromatographic separation was achieved using a reverse phase Kinetex PS C18 2.1*50 mm, 3.5 um, 100A° column under gradient elution with 0.1% formic acid in water and 0.1% formic acid in acetonitrile as mobile phases. The flow rate was 0.6 mL/min, and glyburide was employed as the internal standard (IS). Mass spectrometric detection was performed using positive electrospray ionization mode and multiple reaction monitoring was applied for the quantitative analysis. Protein precipitation with acetonitrile was used for sample preparation. The method demonstrated an excellent linearity range of 1 ng/mL to 1000 ng/mL for both analytes (r2 > 0.99). Intraday and interday accuracy and precision were observed to be within the acceptable regulatory limits for all quality control levels. Considering the limited availability of validated bioanalytical methods for this drug combination, the present work provides a robust and sensitive LC–MS/MS approach for the simultaneous quantification of avutometinib and defactinib. This validated method was successfully applied to a rat pharmacokinetic study following oral administration of both analytes.\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 9","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-07-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148598472","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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