Biomedical Chromatography最新文献_第5页

Investigation Into the Metabolism and Elimination Behavior of RU 58841, and Its Influence on the Steroid Profile in Humans RU 58841的代谢和消除行为及其对人体内类固醇谱影响的研究

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-19 DOI: 10.1002/bmc.70602

Aylin Okutan, Oliver Krug, Gregor Fußhöller, Thomas Piper, Mario Thevis

{"title":"Investigation Into the Metabolism and Elimination Behavior of RU 58841, and Its Influence on the Steroid Profile in Humans","authors":"Aylin Okutan, Oliver Krug, Gregor Fußhöller, Thomas Piper, Mario Thevis","doi":"10.1002/bmc.70602","DOIUrl":"https://doi.org/10.1002/bmc.70602","url":null,"abstract":"<p>RU 58841 is a nonsteroidal antiandrogen, developed for the treatment of androgen-dependent conditions. This study aimed to characterize the human metabolism of RU 58841 for the first time and to assess its systemic exposure following topical administration. In an initial in vitro metabolism study, six potential metabolites were identified using liquid chromatography–high resolution (tandem) mass spectrometry (LC-HRMS/MS). Subsequently, an in vivo administration study was conducted with a RU 58841-containing hair treatment product, applied once to the scalp of six healthy male volunteers. Dried blood spots (DBS) and urine samples were collected and analyzed by LC-low resolution MS/MS. Five in vivo-derived metabolites of RU 58841 were detected in human urine, including products formed via oxidation, N-dealkylation, and glucuronidation of the parent compound and its phase I metabolites. In DBS, the parent compound and the oxidized metabolite were detected, indicating considerable systemic exposure to topically applied RU 58841. The steroid profile (SP) as part of the Athlete Biological Passport (ABP) was not affected by the administration. These findings provide information about the metabolism and the systemic exposure of RU 58841, and further indicate that a single topical dose of 30 mg does not interfere with SP parameter determinations in routine doping controls.</p>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/bmc.70602","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148784899","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

Comparative Characterization of Phytochemicals and In Vivo Metabolites of Aqueous and Ethanol Extracts of Callicarpa nudiflora by UHPLC-Q-TOF-MS/MS and Molecular Networking Combined Multivariate Statistical Methods 用UHPLC-Q-TOF-MS/MS和分子网络结合多元统计方法对海棠花水提物和乙醇提物的化学成分和体内代谢产物的比较研究

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-19 DOI: 10.1002/bmc.70604

Yan Chen, Yu Qi Mei, Xiao Yu Su, Jian Hou, Ke Jian Li, Lin Hou

{"title":"Comparative Characterization of Phytochemicals and In Vivo Metabolites of Aqueous and Ethanol Extracts of Callicarpa nudiflora by UHPLC-Q-TOF-MS/MS and Molecular Networking Combined Multivariate Statistical Methods","authors":"Yan Chen, Yu Qi Mei, Xiao Yu Su, Jian Hou, Ke Jian Li, Lin Hou","doi":"10.1002/bmc.70604","DOIUrl":"https://doi.org/10.1002/bmc.70604","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Callicarpa nudiflora</i> Hook. et Arn. (<i>C. nudiflora</i>), a traditional Chinese medicine, is traditionally used to treat bacterial infections, hepatitis, and hemorrhage. However, its chemical constituents and in vivo metabolic profile have not yet been systematically elucidated, and comparisons of different extracts are still lacking. This study aimed to systematically characterize and compare the in vitro chemical constituents and in vivo metabolites of aqueous (CNW) and ethanol (CNE) extracts of <i>C. nudiflora</i>. A total of 86 chemical constituents were identified in <i>C. nudiflora</i> using UHPLC-Q-TOF-MS/MS combined with molecular networking (MN), including 33 flavonoids, 18 phenylethanoid glycosides, 17 iridoids, 9 phenylpropanoids, 8 terpenoids, and 1 other compound. Based on the identified in vitro constituents and metabolic rules, 12 prototypes and 53 metabolites were further confirmed and annotated in vivo. Furthermore, PCA and OPLS-DA revealed 21 differential in vitro constituents and 16 in vivo compounds between CNW and CNE. These findings indicated that extraction solvent markedly influences the chemical composition and metabolic behavior of <i>C. nudiflora</i>. Overall, this study provides a comprehensive and integrated characterization of phytochemicals and in vivo metabolic profiles of <i>C. nudiflora</i>, offering a robust analytical framework for the comparative evaluation and quality control of different extracts.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148784900","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

Quantitation of Cirtuvivint (SM08502) in Human Plasma by LC–MS/MS LC-MS /MS法定量人血浆中Cirtuvivint (SM08502

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-18 DOI: 10.1002/bmc.70565

Julianne L. Holleran, Joshua J. Deppas, Ye Feng, Michael J. Hochman, Evan C. Chen, Maximilian Stahl, Steven D. Gore, Timothy W. Synold, Jan H. Beumer, Raman Venkataramanan, Robert A. Parise

{"title":"Quantitation of Cirtuvivint (SM08502) in Human Plasma by LC–MS/MS","authors":"Julianne L. Holleran, Joshua J. Deppas, Ye Feng, Michael J. Hochman, Evan C. Chen, Maximilian Stahl, Steven D. Gore, Timothy W. Synold, Jan H. Beumer, Raman Venkataramanan, Robert A. Parise","doi":"10.1002/bmc.70565","DOIUrl":"https://doi.org/10.1002/bmc.70565","url":null,"abstract":"<p>CDC-like kinases (CLK) and dual-specificity tyrosine-regulated kinases (DYRK) are protein kinases involved in various cellular functions, mRNA splicing, and DNA damage repair. CLK/DYRK kinases have been implicated in many disorders such as diabetes, neurodegenerative diseases, and cancer. Cirtuvivint (SM08502) is an orally bioavailable, first-in-class pan-CLK and pan-DYRK inhibitor that modulates pre-mRNA splicing and has shown the ability to inhibit cancer cell growth in vitro and reduce tumor burden in vivo. This has led to the administration of cirtuvivint in phase I clinical trials. To quantitate cirtuvivint, we have developed and validated an LC–MS/MS method in human plasma. The assay is simple and robust and consists of a protein precipitation, dilute-and-shoot extraction method using 20 μL of plasma, chromatographic separation with a Phenomenex Kinetex C18, and a gradient mobile phase system consisting of 0.1% formic acid in water and acetonitrile. The chromatographic method is followed by mass spectrometric detection with a SCIEX 4500 tandem mass spectrometer. The method has a 5-min run time and is linear from 5 to 1000 ng/mL. The assay met the criteria outlined by the US Food and Drug Administration guidance for bioanalytical method validation and will support ongoing and future clinical studies defining cirtuvivint pharmacokinetics.</p>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/bmc.70565","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783603","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

Systematic Characterization of the In Vitro and In Vivo Chemical Constituents of Shenmai Formula by UHPLC-Orbitrap MS 用UHPLC-Orbitrap质谱法系统表征参麦方的体内外化学成分

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-18 DOI: 10.1002/bmc.70598

Xiangying Wang, Jinlian Shen, Jun Qian, Shumin Zhang, Huixin Qiu, Sitong Liu, Mengjie Hong, Xiaodi Kou, Lexin Shu, Yubo Li

{"title":"Systematic Characterization of the In Vitro and In Vivo Chemical Constituents of Shenmai Formula by UHPLC-Orbitrap MS","authors":"Xiangying Wang, Jinlian Shen, Jun Qian, Shumin Zhang, Huixin Qiu, Sitong Liu, Mengjie Hong, Xiaodi Kou, Lexin Shu, Yubo Li","doi":"10.1002/bmc.70598","DOIUrl":"https://doi.org/10.1002/bmc.70598","url":null,"abstract":"<div>\u0000 \u0000 <p>Shenmai Formula (SMF) is a classic traditional Chinese medicine for cardiovascular diseases. Its multicomponent complexity and obscure in vivo metabolic fate hinder understanding of its therapeutic material basis. Because many constituents undergo extensive gastrointestinal and hepatic biotransformation, in vitro profiling alone cannot reveal the actual circulating entities; systematic in vitro–in vivo mapping is therefore essential to define SMF's true bioactive material basis. An in-house constituent database was built from literature (PubMed/CNKI). SMF extract and rat plasma (blank and drug-containing) were analyzed by UHPLC-Orbitrap MS, and constituents were identified by integrating database matching with published literature. Fifty-eight in vitro constituents (mainly saponins) were characterized. Integrating in vitro and in vivo data, 19 circulating prototypes and 14 biotransformed metabolites were mapped in rat plasma. Their biotransformation was driven mainly by deglycosylation, oxidation, methylation, desaturation, and sulfation. The 19 prototypes and 14 metabolites define SMF's in vivo profile and represent the primary potential bioactive candidates for its efficacy. Mapping these active forms and pathways provides a targeted material basis for future pharmacological, pharmacokinetic, and mechanistic studies.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783602","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 Determination of Total and Unbound Amphotericin B by LC–MS/MS: Application to Protein Binding Analysis LC-MS /MS同时测定总和未结合两性霉素B：在蛋白质结合分析中的应用

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-17 DOI: 10.1002/bmc.70600

Min Kan, Fan Yang, Ming-Liang Zhu, Ai-Qing Nie, Jing Xie, Shu-Jing Wang

{"title":"Simultaneous Determination of Total and Unbound Amphotericin B by LC–MS/MS: Application to Protein Binding Analysis","authors":"Min Kan, Fan Yang, Ming-Liang Zhu, Ai-Qing Nie, Jing Xie, Shu-Jing Wang","doi":"10.1002/bmc.70600","DOIUrl":"https://doi.org/10.1002/bmc.70600","url":null,"abstract":"<div>\u0000 \u0000 <p>Amphotericin B (AmB), a first-line antifungal agent, is highly protein-bound, and its efficacy and toxicity are primarily determined by the unbound fraction. However, current therapeutic drug monitoring mainly relies on total plasma concentrations, and clinical data on unbound AmB remain limited. In this study, a rapid and sensitive LC–MS/MS method was developed and validated in accordance with ICH M10 guidelines for the simultaneous quantification of total and unbound AmB concentrations. The method was successfully applied to 52 clinical samples from 26 patients. Correlation analysis combined with locally estimated scatterplot smoothing demonstrated that the protein binding rate (PBR) of AmB was associated with multiple biochemical parameters as well as total drug concentration. Subgroup analyses further revealed significant differences in PBR stratified by total concentration, albumin levels, and eGFR. The method requires only a small plasma volume and shows good applicability in clinical samples, providing a practical tool for investigating unbound pharmacokinetics and supporting individualized therapeutic drug monitoring, particularly in patients with altered protein-binding capacity.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783856","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

Evaluation of Method “Whiteness” in the Stability Analysis of Dexamethasone and PVP-I Ophthalmic Suspensions: Synergizing LC-MS/MS, In Silico Toxicology, and AGREE/GAPI Metrics 地塞米松和PVP-I眼用混悬液稳定性分析中“白度”方法的评价：LC-MS/MS、硅毒理学和AGREE/GAPI指标的协同作用

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-17 DOI: 10.1002/bmc.70590

Likhit Mandal, Praveen Kumar Vemuri, Narender Malothu, Sunil Tiwari

{"title":"Evaluation of Method “Whiteness” in the Stability Analysis of Dexamethasone and PVP-I Ophthalmic Suspensions: Synergizing LC-MS/MS, In Silico Toxicology, and AGREE/GAPI Metrics","authors":"Likhit Mandal, Praveen Kumar Vemuri, Narender Malothu, Sunil Tiwari","doi":"10.1002/bmc.70590","DOIUrl":"https://doi.org/10.1002/bmc.70590","url":null,"abstract":"<div>\u0000 \u0000 <p>This study presents a holistic “White Analytical Chemistry” approach for the stability-indicating evaluation of dexamethasone in complex povidone-iodine (PVP-I) ophthalmic suspensions. Moving beyond traditional validation, the method's “whiteness” was quantitatively assessed via the RGB model, balancing analytical excellence, ecological impact, and operational practicality. The redness (analytical) of the strategy is highlighted by a robust RP-HPLC method integrated with LC-MS/MS for the structural elucidation of degradation products. This was further augmented by in silico toxicological mapping and molecular docking against the human glucocorticoid receptor, providing a comprehensive “risk map” of degradants. The greenness (ecological) was optimized through a design of experiments (DoE) approach and the use of core-shell column technology at a reduced flow rate (0.4 mL/min), achieving an AGREE score of 0.72 and a favorable GAPI profile. The blueness (practicality) was ensured by streamlining the routine analysis for standard UPLC-PDA/UV systems, ensuring cost-effective tech-transfer for high-throughput quality control. Ultimately, this integrative framework provides a superior safety diagnostic tool for complex ophthalmic formulations, aligning high-tier pharmaceutical accuracy with environmental and economic consciousness.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783858","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

QbD-Assisted RP-HPLC Method Development and Validation for the Quantification of Sotagliflozin With LC–MS/MS Characterization of Its Degradation Products and Greenness Assessment Using AGREE and MoGAPI qbd辅助反相高效液相色谱法（LC-MS /MS）建立和验证Sotagliflozin降解产物的表征及使用AGREE和MoGAPI进行绿色评价

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-17 DOI: 10.1002/bmc.70597

Ankit Gupta, Akash Sharma, Gudiya Devi, Chimpiri Srujani, Aswin Viswanath, Desavathu Madhuri, Mastanamma Shaik

{"title":"QbD-Assisted RP-HPLC Method Development and Validation for the Quantification of Sotagliflozin With LC–MS/MS Characterization of Its Degradation Products and Greenness Assessment Using AGREE and MoGAPI","authors":"Ankit Gupta, Akash Sharma, Gudiya Devi, Chimpiri Srujani, Aswin Viswanath, Desavathu Madhuri, Mastanamma Shaik","doi":"10.1002/bmc.70597","DOIUrl":"https://doi.org/10.1002/bmc.70597","url":null,"abstract":"<div>\u0000 \u0000 <p>An AQbD-based approach was employed to develop and validate a reliable, stability-indicating RP-HPLC method for quantifying sotagliflozin in API and tablet dosage forms. Sotagliflozin, a dual SGLT-1/2 inhibitor used in diabetes management and cardiovascular risk reduction, requires a sensitive and robust analytical method for quality control and stability assessment. Critical method parameters were screened using a Taguchi design and optimized through Box–Behnken Design (BBD). Chromatographic separation was achieved on an Agilent Zorbax SB-C18 column using an eco-friendly mobile phase comprising ethanol and 0.1% TFA (pH 2.25) in a 38:62% v/v ratio at a flow rate of 1 mL/min, yielding excellent system performance. The method was validated according to ICH guidelines, demonstrating good linearity (25–150 μg/mL), precision, accuracy, robustness, and sensitivity with low LOD and LOQ values. Forced degradation studies confirmed its stability-indicating capability, with notable degradation under acidic (11.03%), alkaline (14.13%), oxidative (12.39%), and thermal (14.49%) conditions, while minimal degradation occurred under hydrolytic and photolytic stress. LC–MS/MS enabled identification and structural characterization of four major degradation products. Greenness assessment using AGREE and MoGAPI tools yielded scores of 0.89 and 91, respectively, confirming the method's eco-friendly nature for routine pharmaceutical analysis.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783852","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

Metabolomics-Driven Bioactivity-Guided Isolation and Molecular Docking Reveal Antibreast Cancer Metabolome Heterogeneity in Polygonum spp 代谢组学驱动的生物活性引导分离和分子对接揭示蓼属抗乳腺癌代谢组异质性。

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-17 DOI: 10.1002/bmc.70502

Wenjing Zheng, Omar M. Khattab, Qi Yuan, Yajie Wang, Feng Wei, Kaiyu Shen, Houwen Zhang, Xiaoqin Hu, Huiying Fu, Qiyang Shou

{"title":"Metabolomics-Driven Bioactivity-Guided Isolation and Molecular Docking Reveal Antibreast Cancer Metabolome Heterogeneity in Polygonum spp","authors":"Wenjing Zheng, Omar M. Khattab, Qi Yuan, Yajie Wang, Feng Wei, Kaiyu Shen, Houwen Zhang, Xiaoqin Hu, Huiying Fu, Qiyang Shou","doi":"10.1002/bmc.70502","DOIUrl":"10.1002/bmc.70502","url":null,"abstract":"<div>\u0000 \u0000 <p>The rise of triple-negative breast cancer (TNBC) warrants the urgent need to identify novel therapies. Herein, untargeted metabolomics-guided isolation revealed the metabolome fingerprints of <i>Polygonum bistorta</i> (PB) and <i>Polygonum viviparum</i> (PV) in correlation with their TNBC inhibitory activity. Phytochemical analysis annotated 209 metabolites, with flavonoids (45 compounds) as the major class, followed by phenolic acids (25), tannins (24), and hydroxycinnamic acids (18). Multivariate data analysis identified chlorogenic acid, 6-<i>O</i>-galloylarbutin, and procyanidin B1 as key markers of PV, whereas naringenin-<i>O</i>-glucoside, catechin, and crataegunin D characterized PB. Among different polar extracts, ethyl acetate extract of PB (PB-EA) and the <i>n</i>-butanol extract of PV (PV-NB) exhibited the strongest cytotoxicity against 4T1 cells, with IC<sub>50</sub> values of 23.28 ± 0.90 and 39.11 ± 2.36 μg/mL, respectively. Subsequently, the same extracts significantly suppressed tumor growth in the 4T1-Luc orthotopic xenograft mouse model compared with their respective model groups (<i>p</i> < 0.001, <i>p</i> < 0.01). Bioassay-guided isolation yielded 8 compounds, including crataegunin D, which isolated from <i>Polygonaceae</i> plants for the first time, displaying IC<sub>50</sub> values of 24.91 ± 2.43 and 20.65 ± 1.77 μM against 4T1 and MDA-MB-231 cells, respectively. Molecular docking revealed binding free energies (ΔG) ranging from −52 to −48 kcal/mol targeting EGFR and CDK receptors.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148757247","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

In Vivo Evaluation of Coriandrum sativum Extract Against Murine Eimeria papillata Infection and In Silico Analysis of Its Identified Phytochemicals 芫荽提取物抗小鼠乳头状艾美球虫感染的体内评价及其鉴定植物化学物质的硅分析

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-14 DOI: 10.1002/bmc.70596

Abdulsalam Alkhudhayri, Shaimaa M. Kasem, Mohamed A. Dkhil, Heba Ismaeil, Saeed El-Ashram, Kareem A. Abdelmeguid, Felwa A. Thagfan, Nabila M. Mira

{"title":"In Vivo Evaluation of Coriandrum sativum Extract Against Murine Eimeria papillata Infection and In Silico Analysis of Its Identified Phytochemicals","authors":"Abdulsalam Alkhudhayri, Shaimaa M. Kasem, Mohamed A. Dkhil, Heba Ismaeil, Saeed El-Ashram, Kareem A. Abdelmeguid, Felwa A. Thagfan, Nabila M. Mira","doi":"10.1002/bmc.70596","DOIUrl":"https://doi.org/10.1002/bmc.70596","url":null,"abstract":"<div>\u0000 \u0000 <p>Coccidiosis is a protozoan parasitic disease that necessitates sustainable therapeutic alternatives due to increasing resistance to conventional coccidiostats. This study evaluated the anticoccidial efficacy of <i>Coriandrum sativum</i> methanolic extract (CME) against <i>Eimeria papillata</i> infection in mice. Phytochemical profiling of CME was conducted using liquid chromatography–mass spectrometry (LC–MS), and identified compounds were subjected to in silico molecular docking. Twenty-five male Swiss albino mice were divided into the following five groups as follows: Group 1: noninfected, nontreated (control), Group 2: CME administered control, Group 3: infected with <i>E. papillata</i>, Group 4: infected+CME treated group (300 mg/kg), and Group 5: infected+amprolium treated group (120 mg/kg). Mice were orally infected with 1 × 10<sup>3</sup> sporulated oocysts and treated for 5 days. Docking analysis revealed strong binding affinities of several chromatographic CME constituents toward elongation factor Tu (tufA), with docking scores exceeded amprolium's binding affinity. In vivo, CME significantly restored goblet cell counts and upregulated MUC-2 expression. It reduced pathogenic <i>Salmonella typhi</i> and <i>Staphylococcus aureus</i> colonization, downregulated inducible nitric oxide synthase and CD4 expression, enhanced catalase activity, as well as suppressed pro-inflammatory cytokines interleukin-1beta (IL-1β) and tumor necrosis factor-alpha (TNF-α). These findings demonstrate that CME exerts anticoccidial, antioxidant, anti-inflammatory, and culture-based bacterial effects, highlighting its potential as a natural therapeutic agent against murine coccidiosis.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148753743","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

A Rapid and Sensitive LC–MS/MS Method for Quantification of NDSRI in Melatonin Drug Product via Controlled In Situ Formation 一种快速、灵敏的原位可控形成法测定褪黑素制剂中NDSRI含量的LC-MS /MS方法

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2026-08-14 DOI: 10.1002/bmc.70591

Jaya Yalamanchili, Ganja Himavathi, Salakolusu Suresh

{"title":"A Rapid and Sensitive LC–MS/MS Method for Quantification of NDSRI in Melatonin Drug Product via Controlled In Situ Formation","authors":"Jaya Yalamanchili, Ganja Himavathi, Salakolusu Suresh","doi":"10.1002/bmc.70591","DOIUrl":"https://doi.org/10.1002/bmc.70591","url":null,"abstract":"<p>Nitrosamine drug substance–related impurities (NDSRIs) pose a significant safety risk due to their mutagenic and carcinogenic potential, prompting strict regulatory oversight under ICH M7. The propensity for in situ formation of NDSRIs during analytical procedures, particularly in active pharmaceutical ingredients containing reactive amines, emphasizes the need for highly accurate and scrupulously validated methodologies. Melatonin, containing a vulnerable amine, was chosen as a model drug product. A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for quantifying N-Nitroso melatonin. To prevent in situ formation, a scavenger was incorporated during sample preparation. Validation followed regulatory standards, assessing specificity, linearity, accuracy, precision, sensitivity, and robustness. The method showed excellent linearity (1.8–22.5 ng/mL, <i>R</i><sup>2</sup> = 0.9983), sensitivity with LOD of 0.9 ng/mL and LOQ of 1.8 ng/mL, and accuracy with recoveries between 85.3% and 95.9%. Precision was confirmed with %RSD below 2%, whereas robustness testing demonstrated consistent performance under varied conditions. Crucially, the scavenger eliminated false positives by suppressing in situ nitrosamine formation, ensuring data integrity. This validated approach strengthens analytical accuracy and provides a transferable framework for monitoring NDSRIs in other drug products containing reactive amines, supporting regulatory compliance and safeguarding patient health.</p>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-08-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/bmc.70591","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148719327","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