Journal of Chromatography B最新文献

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High-performance thin-layer chromatography combined with effect-directed assays revealed bioactivity profiles of Salvia aegyptiaca, S. verbenaca, and S. officinalis 高效薄层色谱结合效应定向分析揭示了埃及鼠尾草、马鞭草和马鞭草的生物活性谱
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-16 DOI: 10.1016/j.jchromb.2025.124653
Amira Reguigui , Márton Baglyas , Anna Cselőtey , Mehrez Romdhane , Ágnes M. Móricz
{"title":"High-performance thin-layer chromatography combined with effect-directed assays revealed bioactivity profiles of Salvia aegyptiaca, S. verbenaca, and S. officinalis","authors":"Amira Reguigui ,&nbsp;Márton Baglyas ,&nbsp;Anna Cselőtey ,&nbsp;Mehrez Romdhane ,&nbsp;Ágnes M. Móricz","doi":"10.1016/j.jchromb.2025.124653","DOIUrl":"10.1016/j.jchromb.2025.124653","url":null,"abstract":"<div><div>The effect-directed profiling of aqueous ethanol extracts of Tunisian <em>Salvia aegyptiaca</em> and <em>Salvia verbenaca</em> aerial parts and Tunisian and Hungarian <em>Salvia officinalis</em> leaves was achieved by high-performance thin-layer chromatography (HPTLC) coupled with radical scavenging (using DPPH• free radical) and enzyme inhibitory (acetylcholinesterase, AChE) bioactivity assays. The mixture of toluene – ethyl acetate – methanol – formic acid, 11:2:6:1 (<em>V/V</em>) was used as a mobile phase for the separation of bioactive zones. The characterization of the compounds present in the active zones was performed by derivatization with aluminum chloride or natural product-polyethylene glycol (NP-PEG) reagent, and HPTLC–heated electrospray ionization-high resolution tandem mass spectrometry (HPTLC–HESI-HRMS/MS). Compounds in the nine antioxidant zones could be characterized by derivatization as phenolic compounds and tentatively identified by MS as caffeic acid derivatives, or flavonoid glycosides or glucuronides. Rosmarinic acid and luteolin 7-<em>O</em>-glucuronide were detected in <em>S. aegyptiaca</em> and <em>S. officinalis</em> extracts, while apigenin 7-<em>O</em>-glucuronide and luteolin 7-<em>O</em>-glucoside were identified in <em>S. aegyptiaca</em> and <em>S. verbenaca</em>. The co-presence of an unknown caffeic acid derivative, hispidulin 7-<em>O</em>-glucuronide and luteolin 7-<em>O</em>-glucoside was proved within a single zone of <em>S. officinalis</em> extract. Additionally, an unknown rosmarinic acid derivative and an unknown luteolin derivative were detected in <em>S. officinalis</em> and <em>S. verbenaca</em>, respectively. These compounds exhibited weak AChE inhibitory activity, with luteolin 7-<em>O</em>-glucuronide demonstrating the strongest effect.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124653"},"PeriodicalIF":2.8,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144090218","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
Screening and identification of AChE inhibitors from walnut kernel by a combination of bio-affinity ultrafiltration, AChE-functionalized magnetic nanoparticles and UPLC-Q-exactive orbitrap MS 生物亲和超滤、乙酰胆碱功能化磁性纳米颗粒和uplc - q -精确轨道谱联用筛选鉴定核桃仁中乙酰胆碱酯酶抑制剂
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-16 DOI: 10.1016/j.jchromb.2025.124657
Yong Ding , Yu-tong Song , Ze-xu Yang , Xia-jing Xu , Qing-zhu Zhang , Dong-mei Wang , Ying-ni Pan , Kun Ren , Shu-meng Ren , Xiao-qiu Liu
{"title":"Screening and identification of AChE inhibitors from walnut kernel by a combination of bio-affinity ultrafiltration, AChE-functionalized magnetic nanoparticles and UPLC-Q-exactive orbitrap MS","authors":"Yong Ding ,&nbsp;Yu-tong Song ,&nbsp;Ze-xu Yang ,&nbsp;Xia-jing Xu ,&nbsp;Qing-zhu Zhang ,&nbsp;Dong-mei Wang ,&nbsp;Ying-ni Pan ,&nbsp;Kun Ren ,&nbsp;Shu-meng Ren ,&nbsp;Xiao-qiu Liu","doi":"10.1016/j.jchromb.2025.124657","DOIUrl":"10.1016/j.jchromb.2025.124657","url":null,"abstract":"<div><div>Acetylcholinesterase (AChE) is widely concerned as a hotspot target for the treatment of Alzheimer's disease (AD). This study aimed to screen AChE inhibitors from walnut kernel (WK) through the techniques combined of bio-affinity ultrafiltration, AChE-functionalized magnetic nanoparticles and UPLC-Q-Exactive Orbitrap MS. The results showed that WK extract improved acetylcholine level and reduced AChE level in the hippocampus and cortex of AD mice with kidney yang deficiency. AChE inhibition experiment showed WK extract has the best activity with IC<sub>50</sub> values at 1.310 mg/mL. Bio-affinity ultrafiltration combined with UPLC-Q-Exactive Orbitrap MS screened out 3 active compounds, including ellagic acid 4-<em>O</em>-xyloside, ellagic acid (EA) and glansreginin A. In order to avoid false positive results, AChE-functionalized magnetic nanoparticles combined with HPLC was used to ligand fish again, and EA was fished. And the IC<sub>50</sub> value of EA on AChE was 1.486 mg/mL. Molecular docking showed EA had the calculated binding energies at −8.468 kJ/moL with AChE, and could interact with the amino acid residues of ASP 74, TYR 133 and GLU 202 via hydrogen bonds and had the pi-pi bonds with TRP 86. The developed ligand fishing method is simple and efficient for screening potential AChE inhibitors from medicinal plant.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124657"},"PeriodicalIF":2.8,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144098874","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
Development and validation of an LC-MS/MS method for simultaneous determination of XZP-3287(bireociclib) and its metabolites in human plasma, and its clinical pharmacokinetics application LC-MS/MS同时测定人血浆中XZP-3287(bireociclib)及其代谢物的方法建立与验证及其临床药代动力学应用
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-16 DOI: 10.1016/j.jchromb.2025.124658
Bohan Liang , Yanjie Li , Lingmei Xu , Li Wang , Quankun Zhuang , Shiqi Dong , Huirong Fan
{"title":"Development and validation of an LC-MS/MS method for simultaneous determination of XZP-3287(bireociclib) and its metabolites in human plasma, and its clinical pharmacokinetics application","authors":"Bohan Liang ,&nbsp;Yanjie Li ,&nbsp;Lingmei Xu ,&nbsp;Li Wang ,&nbsp;Quankun Zhuang ,&nbsp;Shiqi Dong ,&nbsp;Huirong Fan","doi":"10.1016/j.jchromb.2025.124658","DOIUrl":"10.1016/j.jchromb.2025.124658","url":null,"abstract":"<div><div>XZP-3287(bireociclib) is a novel and selective inhibitor of the cell cyclin-dependent kinases 4/6 (CDK4/6), which is primarily employed for the treatment of breast cancer in clinical trials. In this study, a novel and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous determination of XZP-3287 and its metabolites XZP-5286, XZP-3584 and XZP-5736 in human plasma in accordance with international conference on harmonization of technical requirements for registration of Pharmaceuticals for Human use (ICH) guideline R3 (M10) guideline. The multiple reaction monitoring mode (MRM) of mass spectrometer was used and all compounds were monitored in electrospray ionization (ESI+) mode. The correlation coefficients (R<sup>2</sup>) of all calibration curves for linear regression were greater than 0.99. The intra- and inter-day precision of XZP-3287 and its metabolites XZP-5286, XZP-3584 and XZP-5736 were determined to be 5.2 %–5.5 %, 14.9 %–10.1 %, 6.9 %–13.8 % and 7.3 %–5.6 %, and their accuracy were determined to be 5.2 %–6.0 % 6.9 %–4.4 %, 11.1 %–5.0 % and 7.4 %–5.6 %, respectively. In conclusion, a method for the simultaneous detection of the pharmacokinetic profiles of XZP-3287 and its metabolites in human plasma had been successfully developed. The results demonstrated the efficacy, sensitivity, and reliability of this method</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124658"},"PeriodicalIF":2.8,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144090217","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
Tandem mass tag-based proteomics analysis to reveal growth stage-dependent pathways in Dendrobium nobile Lindl 串联质量标记的蛋白质组学分析揭示了石斛生长阶段依赖性途径
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-16 DOI: 10.1016/j.jchromb.2025.124647
Wanhui Chen , Cong Xie , Wenying He
{"title":"Tandem mass tag-based proteomics analysis to reveal growth stage-dependent pathways in Dendrobium nobile Lindl","authors":"Wanhui Chen ,&nbsp;Cong Xie ,&nbsp;Wenying He","doi":"10.1016/j.jchromb.2025.124647","DOIUrl":"10.1016/j.jchromb.2025.124647","url":null,"abstract":"<div><h3>Objective</h3><div>This study aimed to analyze differentially proteins at various growth stages of <em>Dendrobium nobile Lindl</em> and attempt to find some possible functional proteins related to plant growth or pharmacological activity.</div></div><div><h3>Methods</h3><div>The samples were grouped into two categories based on their growth periods as 2–3 years (S1) and 7–8 years (S2), respectively. Tandem Mass Tag(TMT) labeling-based quantitative proteomics combined LC-MS/MS was applied to identify differential protein expression at various growth stages of <em>Dendrobium nobile</em> Lindl<em>.</em> Those proteins were analyzed by various bioinformatics methods. The activities of several antioxidant enzymes including superoxide dismutase(SOD), peroxidase (POD) and catalase (CAT) in the plant were specifically examined using commercially available assay kits.</div></div><div><h3>Results</h3><div>A total of 6032 proteins were identified with 283 differential proteins related to 168 up-regulated and 115 down-regulated. KEGG pathway enrichment analysis revealed that proteins involved in heat shock response, phenylpropanoid biosynthesis, and antioxidant activity showed significant changes across the growth stages. Specifically, a decrease in small heat shock proteins (sHSPs) was observed in older plants, potentially reducing their stress resilience, while proteins involved in lignin biosynthesis, such as SOD, CAT, and POD, were upregulated, suggesting improved stress response.</div></div><div><h3>Conclusion</h3><div>There are 283 differential proteins with diversiform function between different growth stages. Some upregulated antioxidant enzymes contribute to Dendrobium's ability to combat oxidative stress in older plants. These findings provide insights into how protein expression varies with growth stage, offering scientific support for determining optimal harvesting periods or pharmacological mechanism for <em>Dendrobium nobile</em> Lindl<em>.</em></div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124647"},"PeriodicalIF":2.8,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144084672","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
Optimized plasmid extraction through controlled temperature, prolonged alkaline lysis, and gentle mixing 优化质粒提取通过控制温度,延长碱性裂解,温和混合
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-16 DOI: 10.1016/j.jchromb.2025.124646
Ruijie Hao , Xingyu Li , Ning Wang , Mengzhen Zhang , Min Li , Yongjie Xu , Pengpeng Zhang , Hanling Zhang , Zihan Ma , Bijie Jiang , Xuefeng Wei , Wei Xu
{"title":"Optimized plasmid extraction through controlled temperature, prolonged alkaline lysis, and gentle mixing","authors":"Ruijie Hao ,&nbsp;Xingyu Li ,&nbsp;Ning Wang ,&nbsp;Mengzhen Zhang ,&nbsp;Min Li ,&nbsp;Yongjie Xu ,&nbsp;Pengpeng Zhang ,&nbsp;Hanling Zhang ,&nbsp;Zihan Ma ,&nbsp;Bijie Jiang ,&nbsp;Xuefeng Wei ,&nbsp;Wei Xu","doi":"10.1016/j.jchromb.2025.124646","DOIUrl":"10.1016/j.jchromb.2025.124646","url":null,"abstract":"<div><div>Alkaline lysis serves as an effective technique for plasmid extraction. However, its widespread adoption is significantly impeded by inconsistencies in key technical parameters across different documents. To address these issues, we conducted a rheological behavior analysis to understand the pattern of cell lysis and performed a series of plasmid extraction experiments to determine the optimal technical parameters. The result showed that gentle mixing (inverting tube five times, I5)), extended lysis time (10 min), and elevated lysis temperature (25 °C), each produced the best plasmid preparations, based on plasmid yield, quality, and performance in downstream molecular biology assays. We also discovered that bacterial density influenced cell lysis process. Extending the alkaline lysis duration neither induced resistance to restriction endonuclease (RE) digestion of plasmids nor significantly compromised the integrity of plasmids and host genome; instead, it enhanced the plasmid release. High-frequency and small-amplitude mixing tended to generate more genomic fragments, whereas low-frequency and large-amplitude mixing was likely to result in a higher occurrence of open circular (OC) plasmids. Bacterial lysis at low temperatures (4 °C) could lead to genomic contamination and reduce lysis efficiency. Overall, these findings underscored the importance of technical details and provided guidance for future plasmid extractions.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1262 ","pages":"Article 124646"},"PeriodicalIF":2.8,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144105689","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
Rapid separation and quantification of imidazole dipeptides in meats using a PBr column packed with 3-(pentabromobenzyloxy)propyl group modified silica gel 用3-(五溴苄氧基)丙基修饰硅胶填充的PBr色谱柱快速分离和定量肉类中咪唑二肽
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-16 DOI: 10.1016/j.jchromb.2025.124660
Makoto Ozaki , Tomomi Nakade , Yasunari Yamada , Tsunehisa Hirose , Motoshi Shimotsuma , Shozo Tomonaga
{"title":"Rapid separation and quantification of imidazole dipeptides in meats using a PBr column packed with 3-(pentabromobenzyloxy)propyl group modified silica gel","authors":"Makoto Ozaki ,&nbsp;Tomomi Nakade ,&nbsp;Yasunari Yamada ,&nbsp;Tsunehisa Hirose ,&nbsp;Motoshi Shimotsuma ,&nbsp;Shozo Tomonaga","doi":"10.1016/j.jchromb.2025.124660","DOIUrl":"10.1016/j.jchromb.2025.124660","url":null,"abstract":"<div><div>Meats are rich in imidazole dipeptides (IDPs) such as carnosine, anserine, and balenine, known for their antioxidant and antifatigue properties. The concentrations and types of these IDPs vary significantly among different animal species, necessitating a quantitative method for the precise measurement of individual IDPs. Simultaneous analysis of multiple compounds is typically conducted using reversed-phase high-performance liquid chromatography (RP–HPLC). However, C<sub>18</sub> columns, which are commonly employed in RP–HPLC, fail to adequately retain highly hydrophilic IDPs, making separation and quantification challenging. Previously, we developed a PBr column packed with 3-(pentabromobenzyloxy)propyl group modified silica gel, which effectively retains various highly hydrophilic compounds in RP mode. In this study, we established a method for the rapid separation and quantification of IDPs within 10 min under simplified conditions (isocratic mode) using a single quadrupole liquid chromatography–mass spectrometer (LC–MS) equipped with a PBr column, without the need for derivatization. Linear calibration curves for each IDP were generated using glycyl-L-leucine as the internal standard, with the desolvation temperature of the MS instrument set at 500 °C. The proposed method achieved extraction and recovery rates of IDPs ranging from 100.0 % to 113.5 % at three spiking levels, with no carryover observed, even in samples with high concentrations. Additionally, matrix effects ranged from 95.5 % to 109.6 %, with negligible ion suppression and enhancement effects. Furthermore, the method enabled accurate analysis of IDPs with a relative standard deviation of &lt;15 % in meats from various animal species, including chicken, pork, beef, lamb, mutton, deer, horse, and kangaroo.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1262 ","pages":"Article 124660"},"PeriodicalIF":2.8,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144115950","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
Quantitative GC-NICI-MS and GC-NICI-MS/MS analysis by using isotopologs as internal standards: A tutorial review GC-NICI-MS和GC-NICI-MS/MS以同位素为内标进行定量分析
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-15 DOI: 10.1016/j.jchromb.2025.124648
Dimitrios Tsikas
{"title":"Quantitative GC-NICI-MS and GC-NICI-MS/MS analysis by using isotopologs as internal standards: A tutorial review","authors":"Dimitrios Tsikas","doi":"10.1016/j.jchromb.2025.124648","DOIUrl":"10.1016/j.jchromb.2025.124648","url":null,"abstract":"<div><div>The use of analytes labelled with stable-isotopes of <sup>2</sup>H, <sup>13</sup>C, <sup>15</sup>N, <sup>17</sup>O and/or <sup>18</sup>O, i.e., the isotopologs, as internal standards is unique and considered the <em>Golden Standard</em> is quantitative analyses based on mass spectrometry. However, the handling with isotopologs deserves a great extent of care and attentiveness from the very begin of the analytical process. Many issues need to be considered in order to create an analytical method that generates close-to-reality concentrations of a certain analyte or of group of analytes of the same or different chemical classes in complex biological samples. They including isotopic purity, stability through the entire analytical process including sampling, derivatization, ionization and collision-induced dissociation (CID). The present work deals specifically with the use of isotopologs as internal standards for the quantitative analysis of endogenous and exogenous substances in plasma, serum and urine samples. It focuses on GC–MS and GC–MS/MS, negative-ion chemical ionization (NICI) with methane as the reagent gas, and selected-ion monitoring (SIM) or selected-reaction monitoring (SRM) using argon as the collision gas. Special attention has been paid to purity of isotopologs, cross-contribution of analyte-internal standard, and stability of isotopologs during NICI and CID, to linearity of analyte-isotope detector response upon the analyte concentration. This tutorial review re-examines and discusses exemplarily previously reported validated GC–MS and GC–MS/MS methods, and gives recommendations regarding the handling with stable-isotope labelled analogs in quantitative analyses.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1262 ","pages":"Article 124648"},"PeriodicalIF":2.8,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144105688","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
Quantitative analysis of DNDI-6174 using UPLC-MS/MS: A preclinical target site pharmacokinetic study UPLC-MS/MS定量分析ddi -6174:临床前靶点药代动力学研究
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-15 DOI: 10.1016/j.jchromb.2025.124652
Wietse M. Schouten , Katrien Van Bocxlaer , Hilde Rosing , Alwin D.R. Huitema , Jos H. Beijnen , Jadel M. Kratz , Charles E. Mowbray , Thomas P.C. Dorlo
{"title":"Quantitative analysis of DNDI-6174 using UPLC-MS/MS: A preclinical target site pharmacokinetic study","authors":"Wietse M. Schouten ,&nbsp;Katrien Van Bocxlaer ,&nbsp;Hilde Rosing ,&nbsp;Alwin D.R. Huitema ,&nbsp;Jos H. Beijnen ,&nbsp;Jadel M. Kratz ,&nbsp;Charles E. Mowbray ,&nbsp;Thomas P.C. Dorlo","doi":"10.1016/j.jchromb.2025.124652","DOIUrl":"10.1016/j.jchromb.2025.124652","url":null,"abstract":"<div><div>Leishmaniasis is a neglected parasitic infection that continues to pose a significant global health challenge, with currently limited effective treatment options. DNDI-6174 is a novel orally-active, investigational drug with antileishmanial properties. Herein, a novel ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method was developed and validated to quantify DNDI-6174 in relevant murine biomatrices, <em>i.e.</em>, K<sub>2</sub>EDTA plasma and enzymatically-homogenized skin, spleen and liver to support the translational pharmacokinetic-pharmacodynamic model-informed drug development. The chromatographic system consisted of a gradient elution on a standard C<sub>18</sub> column connected to a triple quadrupole MS, operating in positive ionization mode. Pre-processing of murine tissues with collagenase A led to a superior homogenization and analyte extraction compared to mechanical disruption. Human K<sub>2</sub>EDTA plasma served as a surrogate matrix, enabling accurate (bias between −12.0 % and 9.8 %) and precise (relative standard deviation (RSD) ≤ 12.5 %) quantification of DNDI-6174 in the various murine biomatrices. Sample processing with <em>tert</em>-methylbutyl ether resulted in a reproducible recovery between 70.0 % and 93.8 % (RSD ≤ 4.0 %) with an absolute matrix factor between 0.89 and 1.00 for all biomatrices. DNDI-6174 was stable under various conditions, including under tissue homogenization conditions, in all biomatrices investigated. This method was successfully applied in a translational study using a murine cutaneous leishmaniasis skin infection model to assess the target site pharmacokinetics of DNDI-6174, supporting its development as clinical candidate.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1262 ","pages":"Article 124652"},"PeriodicalIF":2.8,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144124799","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
Quantification of sulbactam and durlobactam in saline and human plasma via ultra-performance liquid chromatography tandem mass spectrometry 超高效液相色谱串联质谱法定量测定生理盐水和人血浆中的舒巴坦和杜氯巴坦
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-14 DOI: 10.1016/j.jchromb.2025.124654
Hanna F. Roenfanz, David P. Nicolau, Joseph L. Kuti
{"title":"Quantification of sulbactam and durlobactam in saline and human plasma via ultra-performance liquid chromatography tandem mass spectrometry","authors":"Hanna F. Roenfanz,&nbsp;David P. Nicolau,&nbsp;Joseph L. Kuti","doi":"10.1016/j.jchromb.2025.124654","DOIUrl":"10.1016/j.jchromb.2025.124654","url":null,"abstract":"<div><div>Sulbactam-durlobactam is a combination β-lactam/β-lactamase inhibitor antibiotic approved in the United States for the treatment of adult patients with hospital-acquired and ventilator-associated bacterial pneumonia due to susceptible isolates of <em>Acinetobacter baumannii-calcoaceticus</em> complex. A liquid chromatography tandem mass spectrometry method for the quantification of sulbactam and durlobactam in human plasma and aqueous matrices has been developed and validated. The standard curves for each drug were linear over the range 0.5 to 50 μg/mL and use the isotopic analogs sulbactam-d<sub>5</sub> and [<sup>13</sup>C<sub>2</sub>, <sup>15</sup>N<sub>2</sub>]-durlobactam as internal standards for their respective analytes. This simple, reproducible method for the determination of sulbactam and durlobactam concentrations was developed with the intent to conduct future pharmacokinetic analyses and to guide clinical laboratories in the development of a therapeutic drug monitoring assay.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124654"},"PeriodicalIF":2.8,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144071200","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
Immobilization of albumin binding domain (ABD) on Sepharose 4B and magnetic particle for efficient single-step purification of human serum albumin 白蛋白结合结构域(ABD)在Sepharose 4B和磁性颗粒上的固定化用于人血清白蛋白的高效一步纯化
IF 2.8 3区 医学
Journal of Chromatography B Pub Date : 2025-05-14 DOI: 10.1016/j.jchromb.2025.124655
Maryam Nazari , Rahman Emamzadeh , Nastaran Masoudi-Khoram , Mahboobeh Nazari
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