Biomedical Chromatography最新文献

Evaluation of Anlotinib Metabolic Stability in HLMs Matrix Applying Ultra-Fast UPLC–MS/MS Approach: Greenness Assessment With In Silico Testing for Structural Alarms Related to the Metabolic Lability and DEREK Toxicity 应用超快速UPLC-MS /MS方法评价Anlotinib在HLMs基质中的代谢稳定性：与代谢不稳定性和DEREK毒性相关的结构报警的绿色度评估与硅测试

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-10-04 DOI: 10.1002/bmc.70231

Mohamed W. Attwa, Ali S. Abdelhameed, Adnan A. Kadi

{"title":"Evaluation of Anlotinib Metabolic Stability in HLMs Matrix Applying Ultra-Fast UPLC–MS/MS Approach: Greenness Assessment With In Silico Testing for Structural Alarms Related to the Metabolic Lability and DEREK Toxicity","authors":"Mohamed W. Attwa, Ali S. Abdelhameed, Adnan A. Kadi","doi":"10.1002/bmc.70231","DOIUrl":"https://doi.org/10.1002/bmc.70231","url":null,"abstract":"<div>\u0000 \u0000 <p>Anlotinib (Focus V) is approved by the China Centre for Drug Evaluation in 2018 as a third-line treatment for patients with certain advanced cancers. This study aimed to develop a specific, fast, reliable, and sustainable ultraperformance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) approach for estimating anlotinib (ANB) in the human liver microsomes (HLMs) matrix, with the application for the assessment of ANB metabolic stability. The validation processes for the UPLC–MS/MS system complied with US Food and Drug Administration regulations following bioanalytical method validation. The established approach was validated using the HLMs matrix over the range of 1.0 to 4000 ng mL<sup>−1</sup> within 1 min. The precision (%RSD) and accuracy (%E) rates for intra-day and inter-day measurements ranged from −6.33% to 4.91% and −6.67% to 5.26%, respectively. The StarDrop software package involved P450 and Deductive Estimation of Risk from Existing Knowledge modules that were applied for assessing metabolic lability and characterizing ANB structural alarms, respectively. The in vitro half-life (<i>t</i><sub>½</sub>) was computed at 44.72 min, while the clearance intrinsic (Cl<sub>int</sub>) of ANB was calculated at 18.13 mL min<sup>−1</sup> kg<sup>−1</sup>. In silico evaluations suggest that minor structural alterations to the methyl group (62%), amine group (37%), and methoxy group (1%) in drug design may increase the ANB metabolic stability.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145224033","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

Detection of Pesticide Residues in Fruits and Vegetables Involving Different Chromatographic Techniques (LC–MS/MS, GC–MS/MS, GC and HPLC) 不同色谱技术（LC-MS /MS、GC - MS/MS、GC和HPLC）在果蔬中农药残留检测中的应用

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-10-04 DOI: 10.1002/bmc.70224

Ishrat Jan, Fehmida Rashied, Naveed A. Malik, Malik Mukhtar, Ramgopal Dudwal, Alka Kataria

{"title":"Detection of Pesticide Residues in Fruits and Vegetables Involving Different Chromatographic Techniques (LC–MS/MS, GC–MS/MS, GC and HPLC)","authors":"Ishrat Jan, Fehmida Rashied, Naveed A. Malik, Malik Mukhtar, Ramgopal Dudwal, Alka Kataria","doi":"10.1002/bmc.70224","DOIUrl":"https://doi.org/10.1002/bmc.70224","url":null,"abstract":"<div>\u0000 \u0000 <p>The rampant use of pesticides in agricultural practices poses significant risks to human health and the environment. To mitigate these risks, regulatory authorities enforce stringent measures to monitor and control pesticide residues in food matrices. Even trace amounts of pesticide residues in various food products, particularly fruits and vegetables, can lead to severe health implications. Consequently, considerable efforts have been directed towards the development of advanced analytical methodologies for the extraction and quantification of pesticide residues. This comprehensive study provides a thorough review of advanced techniques employed in the detection and quantification of pesticide residues in fruits and vegetables. Various instrumental approaches, including gas chromatography coupled with ECD, FPD, NPD, MSD, Q-TOFMS and liquid chromatography combined with UV, DAD, MSD and Q-TOFMS, have been extensively discussed. Each analytical technique offers distinct advantages and limitations in terms of sensitivity, selectivity and applicability to different classes of pesticides. Through an in-depth exploration of these advanced analytical methodologies, this study aims to facilitate a deeper understanding of pesticide residue detection in fruits and vegetables, thereby informing regulatory measures and promoting food safety and public health.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145224026","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

LC–MS/MS–Based Serum Lipidomic Profile to Reveal Cancer-Specific Biomarkers for Renal Cell Carcinoma LC-MS / MS-Based血清脂质组学分析揭示肾细胞癌的癌症特异性生物标志物

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-10-04 DOI: 10.1002/bmc.70230

Lin Lin, Jiaxin Zheng, Sixia Hu

{"title":"LC–MS/MS–Based Serum Lipidomic Profile to Reveal Cancer-Specific Biomarkers for Renal Cell Carcinoma","authors":"Lin Lin, Jiaxin Zheng, Sixia Hu","doi":"10.1002/bmc.70230","DOIUrl":"https://doi.org/10.1002/bmc.70230","url":null,"abstract":"<div>\u0000 \u0000 <p>Renal cell carcinoma (RCC) is one of the most lethal malignant tumors in the urinary system, and its incidence rate is increasing in the last decade. Discovering sensitive and specific biomarkers for RCC and exploring its pathogenesis are of great clinical significance. Here, a liquid chromatography–tandem mass spectrometry (LC–MS/MS) based serum lipidomic profile was carried out to reveal the lipid expression differences in RCC patients and healthy controls. A total of 112 participants were enrolled in the training set, including nonmalignant disease subjects for specific screening. As a result, 66 RCC-specific lipid variables were screened and further validated with an independent test set. Receiver operating characteristic (ROC) analysis was used to evaluate the clinical diagnostic potential of the biomarkers. Twenty-four of them were found to have AUC (area under the curve) values larger than 0.85, and 13 of them were clearly identified. The study indicated reduced lysophosphatidylcholine (LPC) serum levels and increased triglyceride (TG) levels in RCC patients, which might be developed as a potential therapeutic target for cancer treatment. A biomarker pattern composed of TG (19:1/18:2/18:2) and TG (18:0/16:0/16:0) was discovered to have the highest AUC value of 0.995, with a sensitivity and specificity up to 97.6% and 95.0%, respectively.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145224370","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

Comprehensive Analysis of Bioactive Phytoconstituents in Red Flesh of Dioscorea opposita Thunb. by UHPLC-Q-Orbitrap-HRMS 山药红肉中生物活性成分的综合分析。由UHPLC-Q-Orbitrap-HRMS

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-10-04 DOI: 10.1002/bmc.70232

Lanping Yang, Wendi Wang, Zhenzhen Liu, Yangyang Zhai, Zhenhui Wang, Ying Li, Zhenzhen Zhang, Baohua Hou, Baobao Zhang, Jingchun Zhou, Dehong Guo, Miaoqing Zhou, Wei Guo

{"title":"Comprehensive Analysis of Bioactive Phytoconstituents in Red Flesh of Dioscorea opposita Thunb. by UHPLC-Q-Orbitrap-HRMS","authors":"Lanping Yang, Wendi Wang, Zhenzhen Liu, Yangyang Zhai, Zhenhui Wang, Ying Li, Zhenzhen Zhang, Baohua Hou, Baobao Zhang, Jingchun Zhou, Dehong Guo, Miaoqing Zhou, Wei Guo","doi":"10.1002/bmc.70232","DOIUrl":"https://doi.org/10.1002/bmc.70232","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Dioscorea opposita</i> Thunb. cv. Tiegun (DTT) is used daily as food and medicine. However, there is confusion in removing the red flesh of DTT (RF), as the nutrient phytochemicals of RF are unclear. This study aimed to reveal the phytochemicals and antioxidant capabilities of RF. An ultra-high-performance liquid chromatography-quadrupole Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) approach was employed to determine the comprehensive phytochemicals of RF, and the antioxidant activities (DPPH, ABTS, and FRAP) of the extracts were evaluated. A total of 249 phytochemicals were detected, including 150 primary metabolites, 68 secondary metabolites, and 31 other compounds. Notably, 166 differential metabolites (163 upregulated) were identified in RF relative to WF (white flesh). RF significantly increased the contents of primary metabolites (such as lipids, organic acids, and amino acids) and secondary metabolites (such as flavonoids and phenolic acids). RF showed higher antioxidant activity (DPPH, ABTS, and FRAP) than WF. The correlation analysis identified that most of the differential metabolites were significantly positively correlated with the antioxidant capacity. This is the first systematic and comprehensive qualitative analysis of the phytochemicals of RF. This study expands our knowledge of the bioactive constituents of RF and highlights the potential nutritional and medicinal values of DTT.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145224040","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

Metabolic Profile In Vivo and Potential Mechanisms of Danggui Jianzhong Decoction Against Gastric Ulcer by Ultra-High-Performance Quadrupole Time-of-Flight Mass Spectrometry Combined With Network Pharmacology Analysis 当归健中汤抗胃溃疡的体内代谢特征及潜在机制——超高性能四极杆飞行时间质谱联用网络药理学分析

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-10-03 DOI: 10.1002/bmc.70188

Tian-hua Duan, Xiao-ya Jiang, Ze-zhao Zhang, Rong-rong Xu, Rui Li, Xin-guo Wang, Li-ying Niu, Wei Feng

{"title":"Metabolic Profile In Vivo and Potential Mechanisms of Danggui Jianzhong Decoction Against Gastric Ulcer by Ultra-High-Performance Quadrupole Time-of-Flight Mass Spectrometry Combined With Network Pharmacology Analysis","authors":"Tian-hua Duan, Xiao-ya Jiang, Ze-zhao Zhang, Rong-rong Xu, Rui Li, Xin-guo Wang, Li-ying Niu, Wei Feng","doi":"10.1002/bmc.70188","DOIUrl":"10.1002/bmc.70188","url":null,"abstract":"<div>\u0000 \u0000 <p>This study employed an integrated approach that combined ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) with network pharmacology to systematically characterize the phytochemical components and metabolites of Danggui Jianzhong decoction (DGJZD), as well as to elucidate its underlying mechanism. The results showed that a total of 109 compounds were identified. A total of 184 DGJZD-related xenobiotics were screened out in rat bio-samples. Network pharmacology identified 32 active components connecting 25 targets, and the data from the network pharmacology analysis suggested that inflammatory and cancer signaling pathways, EGFR tyrosine kinase inhibitor resistance, PI3K-Akt signaling pathway, and VEGF signaling pathway contribute significantly to the therapeutic effects of DGJZD on gastric ulcer (GU). PTGS2, IL2, PTGS1, PPARG, and EGFR have a high degree and have been proved to have a strong impact on the pathological process. We validated the stable and tight binding of PTGS2, IL2, PTGS1, PPARG, and EGFR with the related core components through molecular docking and molecular dynamics simulation. Taken together, the study clearly gave a comprehensive metabolic profile of DGJZD in vivo first. Our work reveals to study the material basis of the protective effects of DGJZD against GU and the underlying mechanisms.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145211415","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

Liquid Chromatography–Mass Spectrometry Method for the Estimation of Tacrolimus From Whole Blood Using Novel Time Programming Coupled With Diverter Valve Plumbing to Overcome the Matrix Effect 采用新型时间规划耦合分流阀管道的液相色谱-质谱法测定全血中他克莫司的含量以克服基质效应。

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-10-03 DOI: 10.1002/bmc.70227

Sajad Khaliq Dar, Arshad H. Khuroo, Mohd. Akhtar, Pravesh Singh

{"title":"Liquid Chromatography–Mass Spectrometry Method for the Estimation of Tacrolimus From Whole Blood Using Novel Time Programming Coupled With Diverter Valve Plumbing to Overcome the Matrix Effect","authors":"Sajad Khaliq Dar, Arshad H. Khuroo, Mohd. Akhtar, Pravesh Singh","doi":"10.1002/bmc.70227","DOIUrl":"10.1002/bmc.70227","url":null,"abstract":"<div>\u0000 \u0000 <p>Tacrolimus is an immunosuppressant commonly used for the prevention of allograft rejection in transplant patients. Liquid chromatography mass spectrometry (LC–MS/MS) method was successfully developed and validated for the estimation of tacrolimus from whole blood. The extraction of the drug was achieved with protein precipitation followed by solid phase extraction. Tacrolimus related compound A was used as an internal standard. Electrospray ionization in negative mode and multiple reaction monitoring were used to monitor the ion transitions. The method was validated for the linear range of 0.200 ng/mL to 50.000 ng/mL with a correlation coefficient > 0.99. The matrix effect due to whole blood matrix was resolved using an optimized time programming coupled with diverter valve (Valco-valve) plumbing. The developed method was used to estimate tacrolimus concentrations from whole blood in a bioequivalence study. The clinical sample analysis was completed without any failure, and the study was found to be bioequivalent.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145211433","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 Simple and Sensitive HPLC–MS/MS Method for the Simultaneous Quantitative Analysis and Pharmacokinetic Comparison of Four Imidazole-Derived GABA Receptor Agonists: Etomidate, Metomidate, Propoxate, and Isopropoxate in Mouse Blood 一种简单灵敏的HPLC-MS/MS方法用于同时定量分析小鼠血液中四种咪唑衍生的GABA受体激动剂：依托咪酯、美咪酯、丙酸和异丙酸的药代动力学比较。

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-09-28 DOI: 10.1002/bmc.70226

Yuxuan Chen, Xiaolong Zhang, Liyan Sun, Jinlei Liu, Lijie Ma, Mengchao Wang, Yan Shi, Shuo Yang, Jie Gu, Huimin Zhang, Shengnan Zhang, Amin Wurita, Koutaro Hasegawa

{"title":"A Simple and Sensitive HPLC–MS/MS Method for the Simultaneous Quantitative Analysis and Pharmacokinetic Comparison of Four Imidazole-Derived GABA Receptor Agonists: Etomidate, Metomidate, Propoxate, and Isopropoxate in Mouse Blood","authors":"Yuxuan Chen, Xiaolong Zhang, Liyan Sun, Jinlei Liu, Lijie Ma, Mengchao Wang, Yan Shi, Shuo Yang, Jie Gu, Huimin Zhang, Shengnan Zhang, Amin Wurita, Koutaro Hasegawa","doi":"10.1002/bmc.70226","DOIUrl":"10.1002/bmc.70226","url":null,"abstract":"<div>\u0000 \u0000 <p>Etomidate and its structural analogs—metomidate, propoxate, and isopropoxate—have emerged as prevalent substances of abuse in China due to their high addictive potential. This study developed and validated a sensitive, reliable, and high-throughput method using HPLC–MS/MS for simultaneous quantification of four imidazoline-derived new psychoactive substances and the metabolite etomidate acid and then applied it for the molecular pharmacokinetics of five analytes in murine blood. Method validation demonstrated excellent linearity (<i>r</i><sup>2</sup> ≥ 0.999) across calibration curves, with LLOQ ranging from 0.2 to 1 ng/mL and LOD ranging from 0.1 to 0.5 ng/mL. Intraday/interday precision reached 0.123%–11.2%, and accuracy was in the range of −9.68% to 9.86%, which met bioanalytical criteria. Recovery rates (89.3%–103%) and matrix effects (87.1%–105%) were within acceptable ranges. Male KM mice with a body weight of 25 ± 2 g were selected for pharmacokinetic evaluation. Pharmacokinetic analysis revealed significant dose-dependent relationships for maximum plasma concentration (<i>C</i><sub>max</sub>), area under the concentration–time curve (AUC<sub>0–∞</sub>), and detection window (<i>T</i><sub>window</sub>). Metabolic rates followed a descending order: propoxate > isopropoxate > etomidate > metomidate, likely attributed to their lipophilicity gradient. This study systematically elucidates the dose-metabolism kinetics and structure–activity relationships of etomidate analogs, addressing the knowledge gap in toxicokinetic data for propoxate and isopropoxate.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145184473","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

Quantitative Evaluation of the Quality of Shiqi Waigan Granules Based on Fingerprinting and Multi-Indicator Components With Multivariate Statistical Analysis 基于指纹图谱和多指标成分多元统计分析的石芪外肝颗粒质量定量评价

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-09-25 DOI: 10.1002/bmc.70221

Feng Lin, An Yaling, Mei Fang, Xia Tiyu, Jiang Huiling, Peng Lihua, Qiao Weilin, Guo De-an

{"title":"Quantitative Evaluation of the Quality of Shiqi Waigan Granules Based on Fingerprinting and Multi-Indicator Components With Multivariate Statistical Analysis","authors":"Feng Lin, An Yaling, Mei Fang, Xia Tiyu, Jiang Huiling, Peng Lihua, Qiao Weilin, Guo De-an","doi":"10.1002/bmc.70221","DOIUrl":"10.1002/bmc.70221","url":null,"abstract":"<div>\u0000 \u0000 <p>Shiqi Waigan Granules (SWG) are a widely used traditional Chinese medicine for treating common colds, yet a rapid and holistic quality-control protocol has been lacking. In this work, an HPLC fingerprint was built on an Agilent ZORBAX SB-C18 column (4.6 × 250 mm, 5 µm) with acetonitrile–0.1% phosphoric acid gradient elution, 330 nm detection, 40°C column temperature, and 0.6 mL/min flow. Eleven commercial batches were profiled, yielding nine consistent common peaks (similarity > 0.9). Eight of these peaks were unequivocally identified and quantified, all showing excellent linearity (<i>r</i> > 0.9999). Orthogonal partial least-squares discriminant analysis (OPLS-DA) with SIMCA software and variable-importance-in-projection (VIP) scoring highlighted four compounds whose levels differ most among batches and therefore drive product quality. Integrating fingerprinting, quantification, and multivariate statistics thus furnishes a reliable, efficient strategy for routine quality control of Shiqi Waigan Granules.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145136366","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

Pharmacokinetic and Metabolism Study of Ginkgolide C in Rats by UPLC-Q-TOF-MS and UPLC-MS/MS UPLC-Q-TOF-MS和UPLC-MS/MS研究银杏内酯C在大鼠体内的药动学和代谢

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-09-25 DOI: 10.1002/bmc.70223

Yanling Hao, Yuang Zhu, Tiantian Xie, Ping Ye, Bitao Lv

{"title":"Pharmacokinetic and Metabolism Study of Ginkgolide C in Rats by UPLC-Q-TOF-MS and UPLC-MS/MS","authors":"Yanling Hao, Yuang Zhu, Tiantian Xie, Ping Ye, Bitao Lv","doi":"10.1002/bmc.70223","DOIUrl":"https://doi.org/10.1002/bmc.70223","url":null,"abstract":"<div>\u0000 \u0000 <p>Ginkgolide C (GC), a diterpene isolated from <i>Ginkgo biloba</i> leaves, exhibits significant cardiovascular protective activity. The comprehensive pharmacokinetics and metabolic profile of GC in vivo are unknown. In this study, a sensitive and robust LC-MS/MS method was first developed and validated for the determination of GC in rat plasma. The procedure necessitated only 10 μL of rat plasma and involved a protein precipitation process with acetonitrile. Chromatographic separation was achieved on a Waters Acquity UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm) through gradient elution with a mobile phase composed of acetonitrile and water containing 0.1% formic acid. The MS detection was conducted in negative multiple reactions monitoring mode. The method was extensively validated including specificity, sensitivity, intraday and interday accuracy and precision, dilution, carryover, and stability according to the guidelines over the concentration range of 2–5000 ng/mL. The method was subsequently applied to the pharmacokinetic study of GC in rats after intravenous and oral administration. After intravenous administration, GC showed moderate clearance (1816.86 mL/h/kg) with a terminal elimination half-life (<i>t</i><sub>1/2</sub>) of 0.95 h. The volume of distribution (<i>V</i><sub>ss</sub>) is 1038.83 mL/kg. After oral administration at doses of 10, 20, and 40 mg/kg, GC was quickly absorbed into the plasma and reached the peak concentration at 0.5 h. The systemic exposure of GC increased with dose dependent up to 40 mg/kg with low oral bioavailability (4.91%–6.80%). In addition, a total of 14 metabolites were detected and identified in rat plasma, urine, and feces. The biotransformation pathways were tentatively identified as oxidation, dehydrogenation, hydrogenation, hydrolysis, methylation, and sulfate conjugation. The pharmacokinetics and metabolic characteristics of GC were expounded in this study, which provided a solid foundation for in-depth development.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145146517","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

Development and Validation of a Rapid and Simple UHPLC–MS/MS Method for the Determination of Colchicine in Human Plasma 高效液相色谱-质谱联用/质谱联用测定人血浆中秋水仙碱的方法建立及验证

IF 1.7 4区医学

Biomedical Chromatography Pub Date : 2025-09-23 DOI: 10.1002/bmc.70222

Nela Žideková, Kristián Pršo, Marek Pršo, Miloš Jeseňák, Oldřich Farsa, Martin Kertys

{"title":"Development and Validation of a Rapid and Simple UHPLC–MS/MS Method for the Determination of Colchicine in Human Plasma","authors":"Nela Žideková, Kristián Pršo, Marek Pršo, Miloš Jeseňák, Oldřich Farsa, Martin Kertys","doi":"10.1002/bmc.70222","DOIUrl":"10.1002/bmc.70222","url":null,"abstract":"<p>Colchicine is a naturally occurring alkaloid primarily derived from plants of the Colchicum genus, which is used to treat gout and serve as a frontline therapy for various inflammatory conditions, including familial Mediterranean fever. Although it is not recommended for routine therapeutic drug monitoring, there are situations where it may be beneficial, such as in dose adjustments. The present study introduces an LC–MS/MS method for quantifying colchicine in human plasma. A one-step extraction procedure employing an Ostro plate was applied, and the extracts were analyzed using gradient elution followed by detection on a mass spectrometer in multiple reaction monitoring mode. Our method offers several advantages, including a low sample volume and a run time of only 3 min. It demonstrates sufficient linearity to quantify low and high concentrations of colchicine in human plasma samples. The method was successfully validated in accordance with the ICH guideline M10 on bioanalytical method validation, covering selectivity, linearity, limit of quantification, accuracy, precision, dilution integrity, carry-over effect, matrix effects, extraction recovery, and stability over a concentration range of 0.05–100 ng/mL. The fully developed and validated method was applied to determine colchicine in plasma samples from patients diagnosed with familial Mediterranean fever.</p>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 11","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/epdf/10.1002/bmc.70222","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145129316","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