Journal of pharmaceutical and biomedical analysis最新文献_第3页

Bushen Huoxue formula attenuates recurrent spontaneous abortion by modulating arginine metabolism and macrophage polarization at the maternal-fetal interface 补肾活血方通过调节母胎界面的精氨酸代谢和巨噬细胞极化，减轻复发性自然流产。

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-24 DOI: 10.1016/j.jpba.2025.117161

Jingyi Song , Yuan Xu , Jihong Liu , Yuqing Zhong , Ying Hong , Shiqi Liu , Xiaojun Gou , Yan Wu , Quanfang Jin

{"title":"Bushen Huoxue formula attenuates recurrent spontaneous abortion by modulating arginine metabolism and macrophage polarization at the maternal-fetal interface","authors":"Jingyi Song , Yuan Xu , Jihong Liu , Yuqing Zhong , Ying Hong , Shiqi Liu , Xiaojun Gou , Yan Wu , Quanfang Jin","doi":"10.1016/j.jpba.2025.117161","DOIUrl":"10.1016/j.jpba.2025.117161","url":null,"abstract":"<div><div>The aim of this study was to clarify the effects of BSHXF on pregnancy outcome and macrophage polarization at the maternal-fetal interface in a mouse model of recurrent spontaneous abortion (RSA). The RSA model was established using the CBA/J × DBA/2 mating method. Network pharmacology predicted the mechanism of BSHXF intervention in RSA and verified by Western blotting. Immunofluorescence and RT-qPCR were used to measure the levels of macrophage-associated cytokines at the maternal-fetal interface. Placental metabolomics was used to analyze the mechanism of macrophage regulation by BSHXF and verified by ELISA. BSHXF improved embryonic resorption and hormone levels in RSA mice and restored abnormal NF-κB signaling, which was achieved in part by modulating macrophage polarisation status. BSHXF intervention decreased M1 macrophage polarization while elevating M2 macrophage levels. Metabolomics indicated that decreased inducible nitric oxide synthase (iNOS) pathway and elevated arginase-1 pathway (Arg-1) pathway in the placenta were the key mechanisms of macrophage polarization. This study provides innovative insights into the mechanism by which BSHXF ameliorates RSA in mice, providing a scientific basis for further pharmacological research.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117161"},"PeriodicalIF":3.1,"publicationDate":"2025-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145199803","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Determination of methylene blue and detection of its demethylated metabolites in blood plasma using micellar electrokinetic chromatography with UV detection 胶束电动色谱-紫外检测法测定血浆中亚甲基蓝及其去甲基化代谢物

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-23 DOI: 10.1016/j.jpba.2025.117155

Alexander Vladimirovich Ivanov , Valery Vasil’evich Aleksandrin , Polina Alexandrovna Pudova , Maria Pavlovna Galdobina , Alexander Gennadievich Filippov , Mikhail Aleksandrovich Popov , Ruslan Andreevich Maslennikov , Aslan Amirkhanovich Kubatiev

{"title":"Determination of methylene blue and detection of its demethylated metabolites in blood plasma using micellar electrokinetic chromatography with UV detection","authors":"Alexander Vladimirovich Ivanov , Valery Vasil’evich Aleksandrin , Polina Alexandrovna Pudova , Maria Pavlovna Galdobina , Alexander Gennadievich Filippov , Mikhail Aleksandrovich Popov , Ruslan Andreevich Maslennikov , Aslan Amirkhanovich Kubatiev","doi":"10.1016/j.jpba.2025.117155","DOIUrl":"10.1016/j.jpba.2025.117155","url":null,"abstract":"<div><div>A new approach to the direct determination of the drug methylene blue (MB) in blood plasma was developed based on MEKC. We used liquid-phase extraction with acetonitrile and dichloromethane and solid-phase extraction on a strong cation exchange sorbent to extract the analyte from the matrix. Using UV detection (292 nm) and a 50 μm internal diameter silica capillary with a total length of 38 cm (31.5 cm effective) filled with 40 mM phosphate Na, 150 mM SDS, 5 % (v/v) isopropanol, and 12 % (v/v) n-butanol (pH 2.06), an LOD of 5.8 ng/mL for MB and a total analysis time of 16.5 min were obtained. The accuracy was 97.4–103 %, and intra- and interday imprecision were 5.7 and 2.5 %, respectively. This approach was tested on blood samples from rats that were injected with MB. The developed approach also allows for the detection of demethylated MB metabolites (azure A and azure B) and is suitable for the analysis of organs (the brain, liver, and kidneys).</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117155"},"PeriodicalIF":3.1,"publicationDate":"2025-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145155332","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Discovery of chemical markers for maidong (roots of Ophiopogon japonicus and Liriope spicata): A feature-based molecular networking approach 麦冬和麦冬根化学标记的发现：基于特征的分子网络方法。

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-22 DOI: 10.1016/j.jpba.2025.117158

Feiyi Lei , Laurent Bigler , Caroline Weckerle , Luiz Leonardo Saldanha

{"title":"Discovery of chemical markers for maidong (roots of Ophiopogon japonicus and Liriope spicata): A feature-based molecular networking approach","authors":"Feiyi Lei , Laurent Bigler , Caroline Weckerle , Luiz Leonardo Saldanha","doi":"10.1016/j.jpba.2025.117158","DOIUrl":"10.1016/j.jpba.2025.117158","url":null,"abstract":"<div><div>Tuberous roots of <em>Ophiopogon japonicus</em> and <em>Liriope spicata</em> are collectively used as <em>maidong</em> medicine in China for the same clinical efficacy, nourish <em>yin</em> and generate fluids, moisten lung, and clear heart fire. Extensive cultivation of these species has led to the need for more robust quality assessments. Nevertheless, few studies have characterized the metabolomic profile specific to species and growing regions, with a particular focus on their active compounds. A comprehensive understanding of metabolomic profiles of <em>maidong</em> is essential to guide quality control efforts effectively. Therefore, an untargeted metabolomics profiling approach was conducted using ultra-high performance liquid chromatography coupled to a timsTOF Pro hybrid quadrupole-time-of-flight mass spectrometer. Compounds were annotated using an integrated approach based on feature-based molecular networking (FBMN) together with <em>in silico</em> and experimental spectra databases comparisons. The present study showcases a holistic overview of the metabolomic diversity and variation among <em>maidong</em> derived from different origins. Steroidal saponins and homoisoflavonoids were recognized as predominant chemical classes in <em>L. spicata</em>, and <em>O. japonicus</em>, respectively. Characteristic metabolites among <em>maidong</em> derived from four origins were highlighted. Annotations of 58 metabolites revealed significant inter-species discrimination, with 6 and 36 metabolites critical for regional differentiation in <em>L. spicata</em> and <em>O. japonicus</em>, respectively. This approach supports the advancement of quality control strategies for botanical medicines, particularly those derived from multiple origins, ensuring a more rigorous chemical marker selection for botanical medicines.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117158"},"PeriodicalIF":3.1,"publicationDate":"2025-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145185905","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Design of an electrochemical sensor based on molecularly imprinted polymers for sensitive and selective detection of the JAK inhibitor baricitinib 基于分子印迹聚合物的电化学传感器的设计，用于JAK抑制剂baricitinib的灵敏和选择性检测。

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-22 DOI: 10.1016/j.jpba.2025.117154

Ahmed Isa , Egita Banevičiūtė , Ensar Piskin , Ahmet Cetinkaya , Esen Bellur Atici , Almira Ramanaviciene , Sibel A. Ozkan

{"title":"Design of an electrochemical sensor based on molecularly imprinted polymers for sensitive and selective detection of the JAK inhibitor baricitinib","authors":"Ahmed Isa , Egita Banevičiūtė , Ensar Piskin , Ahmet Cetinkaya , Esen Bellur Atici , Almira Ramanaviciene , Sibel A. Ozkan","doi":"10.1016/j.jpba.2025.117154","DOIUrl":"10.1016/j.jpba.2025.117154","url":null,"abstract":"<div><div>Baricitinib (BAR), a selective JAK1/JAK2 inhibitor, is a widely used drug in the treatment of inflammatory and immune-related disorders, including rheumatoid arthritis and COVID-19 complications. However, due to its narrow therapeutic index and pharmacokinetics, precise therapeutic drug monitoring is necessary. While HPLC-based methods are commonly employed, they tend to suffer from high costs, lengthy analysis, and complex procedures. Electrochemical methods offered a promising alternative, but selectivity remains a challenge in biological matrices. To address this, a highly sensitive and selective molecularly imprinted polymer (MIP)-based electrochemical sensor (poly(Py-co-2-TBA)/BAR@MIP/GCE sensor) for BAR detection was developed in this study. The sensor was fabricated using the electropolymerization (EP) technique on a glassy carbon electrode, utilizing 2-phenylboronic acid (2-TBA) as the functional monomer and pyrrole (Py) to provide both conductivity and stability to the polymeric structure. Key parameters, including template-to-monomer ratio, polymerization cycles, and rebinding time, were optimized. Electrochemical and surface morphology characterizations were performed using electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and scanning electron microscopy (SEM). The sensor demonstrated excellent selectivity for BAR, even in the presence of structurally similar compounds. The developed MIP-based sensor presents a cost-effective, rapid, and reliable tool for BAR monitoring, supporting personalized dosing and improved therapeutic outcomes.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117154"},"PeriodicalIF":3.1,"publicationDate":"2025-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145149652","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Characterizing recombinant protein and its fragmentation by top-down mass spectrometry 自上而下质谱法表征重组蛋白及其片段化

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-22 DOI: 10.1016/j.jpba.2025.117157

Zhen Long , Dening Pei , Xiang Zhu , Weijing Liu , Xi Luo , Wenhong Fan , Lei Tao

{"title":"Characterizing recombinant protein and its fragmentation by top-down mass spectrometry","authors":"Zhen Long , Dening Pei , Xiang Zhu , Weijing Liu , Xi Luo , Wenhong Fan , Lei Tao","doi":"10.1016/j.jpba.2025.117157","DOIUrl":"10.1016/j.jpba.2025.117157","url":null,"abstract":"<div><div>This study establishes a top-down mass spectrometry method for evaluating the structural integrity and fragmentation profiles of recombinant proteins. Three representative samples were analyzed: recombinant collagen 1 (RC1, 15.037 kDa; no disulfide bonds), recombinant collagen 2 (RC2, 49.859 kDa; no disulfide bonds), and interferon α2b (19.497 kDa; two disulfide bonds). Both targeted MS²-based, and data-dependent acquisition (DDA)-based top-down workflows were established to accommodate different analytical needs. The developed top-down strategies enabled direct sequencing of proteins with highly repetitive sequences, which pose challenges for bottom-up methods. The findings of this study provide insights into the identification of proteins with molecular weights (MWs) below 50 kDa. First, for proteins with MWs below 12 kDa, DDA-based top-down analysis utilizing HCD fragmentation provides high-throughput identification with 50 % (eg. of 27 fragments for protein RC1). Second, for proteins with MWs greater than 12 kDa, target-MS<sup>2</sup>-based top-down approaches improve sequence coverage, achieving up to 49.5 % for RC2 by combining three dissociation strategies. Third, for proteins containing disulfide bonds, disulfide reduce pretreatment prior to MS analysis is necessary to achieve improved residue cleavage coverage. Overall, this work demonstrates that top-down mass spectrometry provides complementary data to bottom-up methods, delivering crucial insights for comprehensive characterization of therapeutic recombinant proteins.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117157"},"PeriodicalIF":3.1,"publicationDate":"2025-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145155331","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Oxysterol fingerprinting via UPLC-APCI-MS/MS for monitoring developmental stages in the zebrafish model UPLC-APCI-MS/MS技术在斑马鱼模型发育阶段的应用。

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-22 DOI: 10.1016/j.jpba.2025.117156

Francesco Della Valle , Fabiola Eugelio , Carmine Merola , Giulia Caioni , Federico Fanti , Marcello Mascini , Antonella Damiano , Michele Amorena , Michele Del Carlo , Manuel Sergi , Dario Compagnone

{"title":"Oxysterol fingerprinting via UPLC-APCI-MS/MS for monitoring developmental stages in the zebrafish model","authors":"Francesco Della Valle , Fabiola Eugelio , Carmine Merola , Giulia Caioni , Federico Fanti , Marcello Mascini , Antonella Damiano , Michele Amorena , Michele Del Carlo , Manuel Sergi , Dario Compagnone","doi":"10.1016/j.jpba.2025.117156","DOIUrl":"10.1016/j.jpba.2025.117156","url":null,"abstract":"<div><div>Oxysterols, oxidized derivatives of cholesterol, play multifaceted roles in cholesterol homeostasis and cellular signalling. Despite their recognized biological relevance, the temporal dynamics of oxysterol profiles during vertebrate development remain poorly understood. In this study, we developed and validated a robust UHPLC-MS/MS method for the quantification of ten oxysterols in zebrafish (Danio rerio) embryos across five developmental stages (3-, 24-, 48-, 72-, and 96-hours post-fertilization). The method exhibited excellent performance in terms of sensitivity, recovery, and reproducibility, following EMA guidelines. A combination of hierarchical clustering analysis (HCA) and Random Forest classification revealed distinct stage-specific oxysterol profiles. Notably, 6α-hydroxycholesterol emerged as the most discriminative marker, followed by 24- and 27-hydroxycholesterol, indicating their potential involvement in neurodevelopmental and metabolic regulation processes. These findings provide new insights into the role of oxysterols during embryogenesis and establish a reliable platform for evaluating oxysterol dynamics in developmental, toxicological, and pharmacological studies using the zebrafish model.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117156"},"PeriodicalIF":3.1,"publicationDate":"2025-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145206711","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Adaptive wavenumber selection framework for medicine authenticity assessment 药品真实性评估的自适应波数选择框架

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-22 DOI: 10.1016/j.jpba.2025.117153

Fábio do Prado Puglia , Michel J. Anzanello , Marco Flôres Ferrão , Rafael Scorsatto Ortiz , Kristiane Mariotti , Ânderson Ramos Carvalho

{"title":"Adaptive wavenumber selection framework for medicine authenticity assessment","authors":"Fábio do Prado Puglia , Michel J. Anzanello , Marco Flôres Ferrão , Rafael Scorsatto Ortiz , Kristiane Mariotti , Ânderson Ramos Carvalho","doi":"10.1016/j.jpba.2025.117153","DOIUrl":"10.1016/j.jpba.2025.117153","url":null,"abstract":"<div><div>The proliferation of counterfeit medicines presents a critical challenge to global health. ATR-FTIR spectroscopy offers a rapid and efficient means of analyzing these products, but the high dimensionality of spectral data requires effective wavenumber selection. This paper introduces a novel two-step adaptive wavenumber selection framework for classifying authentic and falsified medicines. The method initially partitions spectral data into intervals based on class distance, followed by an iterative ranking process that integrates both wavenumber relevance and redundancy. By penalizing correlated features, our approach avoids redundant information and identifies optimal wavenumber combinations. When applied to the Cialis dataset, the proposed approach achieved near-perfect accuracy (99.97 %), retaining only 2.9 wavenumbers; as for the Viagra dataset, the method achieved 98.73 % accuracy while retaining a subset of 12.4 wavenumbers. Compared to the relevance-only alternative approach, our method retained significantly fewer wavenumbers across all classifiers while consistently achieving comparable or even higher classification performance.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117153"},"PeriodicalIF":3.1,"publicationDate":"2025-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145155333","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A rapid CRISPR-Cas12a/T7EI integrated workflow for high-throughput screening of homozygous mutant cell lines 一种快速CRISPR-Cas12a/T7EI集成工作流程，用于高通量筛选纯合突变细胞系

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-21 DOI: 10.1016/j.jpba.2025.117152

Guohui Xiao , Hongyu Shi , Qiao Lin , Siqi Li , Junyan He , Guoliang Zhang

{"title":"A rapid CRISPR-Cas12a/T7EI integrated workflow for high-throughput screening of homozygous mutant cell lines","authors":"Guohui Xiao , Hongyu Shi , Qiao Lin , Siqi Li , Junyan He , Guoliang Zhang","doi":"10.1016/j.jpba.2025.117152","DOIUrl":"10.1016/j.jpba.2025.117152","url":null,"abstract":"<div><div>Efficient screening for homozygous mutant cell lines, particularly those resulting from low-efficiency CRISPR-Cas9 editing, remains challenging. Here, we developed HomoSelect-CT, an integrated workflow combining CRISPR-Cas12a nucleic acid detection with T7 Endonuclease I (T7EI) genotyping, designed to streamline the screening process for homozygous mutant cell lines. This method requires no specialized instrumentation, enhancing accessibility and efficiency. We validated HomoSelect-CT by successfully identifying homozygous mutants in CRISPR-Cas9-edited THP-1 cells, which was confirmed by Sanger sequencing and Western blot (WB). These findings demonstrate that HomoSelect-CT is a robust and efficient alternative for the rapid isolation of genome-edited cell lines. The entire screening workflow, from monoclonal cultures to confirmed homozygous mutants, is completed in under 4 h, requiring only standard PCR equipment and routine reagents. Thus, HomoSelect-CT represents a significant advancement in CRISPR screening methodology, offering remarkable simplicity and enabling high-throughput screening that is particularly suitable for mutants arising from low-efficiency editing events.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117152"},"PeriodicalIF":3.1,"publicationDate":"2025-09-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145118388","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

LC-MS/MS method for quantification of avacopan in human plasma from patients treated for antineutrophil cytoplasmic antibody-associated vasculitis LC-MS/MS方法定量抗中性粒细胞细胞质抗体相关血管炎患者血浆中阿伐柯潘的含量

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-20 DOI: 10.1016/j.jpba.2025.117151

Juliette Blondel , Léo Froelicher-Bournaud , Stanislas Faguer , Jean Philippe Coindre , Benjamin Terrier , Michel Vidal , Xavier Declèves , Alicja Puzskiel , Benoit Blanchet

{"title":"LC-MS/MS method for quantification of avacopan in human plasma from patients treated for antineutrophil cytoplasmic antibody-associated vasculitis","authors":"Juliette Blondel , Léo Froelicher-Bournaud , Stanislas Faguer , Jean Philippe Coindre , Benjamin Terrier , Michel Vidal , Xavier Declèves , Alicja Puzskiel , Benoit Blanchet","doi":"10.1016/j.jpba.2025.117151","DOIUrl":"10.1016/j.jpba.2025.117151","url":null,"abstract":"<div><div>Avacopan is a new treatment for antineutrophil cytoplasmic antibody-associated vasculitis (ANCA-AAV). To date, there has been a lack of published bioanalytical methods to assay it in plasma, resulting in sparse pharmacokinetic data in clinical settings. The objective of this study was to develop and validate a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the quantification of avacopan in human plasma. [<sup>2</sup>H<sub>4</sub>]-Avacopan was as used as internal standard (IS). Samples were prepared by protein precipitation and separated was on an Accurore® C18 column (2.1 ×50 mm, 2.6 µm), with an elution gradient at a flow rate of 0.5 mL/min. The mobile phase consisted of acetonitrile (0.1 % formic acid) and water (0.1 % formic acid). The analysis run time was 6 min. Avacopan was detected by electrospray ionization on a TSQ Quantis® triple quadrupole mass spectrometer (ThermoFisher Scientific). The linearity of method ranged from 10 to 800 ng/mL. The within-run and between-run relative standard deviations were < 10.2 %. The within-run and between-run relative errors ranged from 2.4 % to 14.4 %. The IS-normalized matrix effect ranged from 2.2 % to 5.1 %, and the IS-normalized extraction recovery ranged from 104.3 % to 109.7 %. The method was fully validated, including checks on linearity, dilution integrity and carry-over. Plasma samples from 16 patients undergoing treatment for ANCA-AAV were then successfully treated with the method. The reanalysis of the samples incurred was below 14 %. This method is suitable for plasma drug monitoring of avacopan because it is both accurate and precise, and meets all validation criteria.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117151"},"PeriodicalIF":3.1,"publicationDate":"2025-09-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145118389","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A UHPLC-Q/TOF-MS/MS-based systematic strategy for analysis of chemical constituents and rat metabolite profiles of modified Shengmai powder 基于UHPLC-Q/TOF-MS/ ms的改良生脉散化学成分及大鼠代谢物分析方法

IF 3.1 3区医学

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-17 DOI: 10.1016/j.jpba.2025.117150

Meng Zhou , Huizhi Luo , Jingjing Ding , Qi Lv , Wanyue She , Jueying Wang , Xiquan Xu , Maidina Aimurula , Changyin Li , Rong Sun , Liyuan Tian , Yu Gu

{"title":"A UHPLC-Q/TOF-MS/MS-based systematic strategy for analysis of chemical constituents and rat metabolite profiles of modified Shengmai powder","authors":"Meng Zhou , Huizhi Luo , Jingjing Ding , Qi Lv , Wanyue She , Jueying Wang , Xiquan Xu , Maidina Aimurula , Changyin Li , Rong Sun , Liyuan Tian , Yu Gu","doi":"10.1016/j.jpba.2025.117150","DOIUrl":"10.1016/j.jpba.2025.117150","url":null,"abstract":"<div><div>Modified Shengmai Powder (MSP), derived from a classical formula in <em>Yixue Qiyuan</em>, has demonstrated clinical efficacy in alleviating radiation-induced injuries. However, its holistic chemical constituents and <em>in vivo</em> bioactive constituents remain unclear. In this study, a systematic strategy based on ultra-high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q/TOF-MS/MS) combined with the MS-DIAL and MS-FLO platforms was developed to analyze the chemical constituents of MSP and its metabolite profiles in rats. As a result, a total of 121 chemical constituents in MSP were identified, including 33 phenylpropanoids, 21 terpenes, 18 flavonoids, 14 saponins, 11 organic acids, 10 glycosides, 5 amino acids, 2 sugars, and 7 others. Chlorogenic acid was identified as the predominant constituent and was recommended as a key quality marker. Furthermore, 38 prototype constituents and 47 metabolites were identified in serum, urine, and feces of rats. It was also observed that metabolic pathways primarily involved phase I processes, mainly including oxidation, reduction, and hydrolysis, while phase II pathways and their associated metabolites were relatively less prominent. In conclusion, this study identified the chemical constituents of MSP and characterized their metabolite profiles in rat serum, urine and feces. These findings provide a scientific basis for further exploration of the material basis underlying MSP efficacy and offer theoretical support for understanding its mechanism of action and clinical applications.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"267 ","pages":"Article 117150"},"PeriodicalIF":3.1,"publicationDate":"2025-09-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145105794","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0