Journal of Chromatography B最新文献_第7页

MOF-199@ tryptophan coated on magnetic bar for stir-bar sorptive extraction of warfarin and aspirin from biological samples followed by quantification through HPLC-UV 磁棒包被MOF-199@色氨酸用于搅拌棒吸附提取生物样品中的华法林和阿司匹林，并通过高效液相色谱-紫外定量。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-29 DOI: 10.1016/j.jchromb.2025.124877

Parastoo Fouladi , Milad Ghani , Jahan Bakhsh Raoof

Tryptophan-functionalized MOF-199 was synthesized via a simple solvothermal method and employed as a novel sorbent for the development of stir-bar sorptive extraction (SBSE) method. The extraction efficiency of the SBSE method was systematically investigated using warfarin and aspirin as model compounds. The extracted drugs were analyzed using high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Key parameters affecting SBSE, including stirring rate, desorption solvent, pH, extraction and desorption time, and salt concentration, were optimized, resulting in 800 rpm stirring rate, 5 min extraction, 1 min desorption, 11 % (w/v) salt concentration, 100.0 μL desorption solvent, and pH = 3.0 as optimal condition. Under the condition, the method exhibited excellent linearity (0.10–200.00 μg L⁻¹ for aspirin and 0.10–100.00 μg L⁻¹ for warfarin), low limits of detection (0.04 and 0.03 μg L⁻¹) and limits of quantification (0.13 and 0.09 μg L⁻¹), and satisfactory precision (%RSD = 4.40–7.60 % for aspirin and 5.10–6.50 % for warfarin). Enrichment factors (EFs) of 56.00 and 64.00 were achieved for aspirin and warfarin, respectively. The proposed SBSE-HPLC-UV method was successfully applied to biological samples, including plasma and urine, demonstrating high reproducibility, efficiency, and suitability for trace-level drug analysis. These results highlight the potential of tryptophan-functionalized MOF-199 as an effective sorbent for analytical applications in pharmaceutical and biological matrices. The method was further evaluated using the Blue Applicability Grade Index (BAGI), achieving a score of 82.5.

采用简单的溶剂热法合成了色氨酸功能化MOF-199，并将其作为一种新型吸附剂用于搅拌棒吸附萃取（SBSE）方法的开发。以华法林和阿司匹林为模型化合物，系统考察了SBSE法的提取效率。采用高效液相色谱-紫外检测（HPLC-UV）对提取的药物进行分析。对影响SBSE的搅拌速率、解吸溶剂、pH、萃取和解吸时间、盐浓度等关键参数进行了优化，结果表明：搅拌速率为800 rpm，萃取时间为5 min，解吸时间为1 min，盐浓度为11% (w/v)，解吸溶剂为100.0 μL, pH = 3.0为最佳条件。在此条件下，该方法具有良好的线性（阿司匹林为0.10 ~ 200.00 μ L-1，华法林为0.10 ~ 100.00 μ L-1）、低检出限（0.04、0.03 μ L-1）和定量限（0.13、0.09 μ L-1），精密度（%RSD = 4.40 ~ 7.60%，华法林为5.10 ~ 6.50%）。阿司匹林和华法林的富集因子（EFs）分别为56.00和64.00。该方法成功地应用于生物样品，包括血浆和尿液，具有高重现性、高效率和痕量药物分析的适用性。这些结果突出了色氨酸功能化MOF-199作为一种有效的吸附剂在药物和生物基质分析中的应用潜力。采用蓝色适用性等级指数（BAGI）对该方法进行进一步评价，得分为82.5分。

{"title":"MOF-199@ tryptophan coated on magnetic bar for stir-bar sorptive extraction of warfarin and aspirin from biological samples followed by quantification through HPLC-UV","authors":"Parastoo Fouladi , Milad Ghani , Jahan Bakhsh Raoof","doi":"10.1016/j.jchromb.2025.124877","DOIUrl":"10.1016/j.jchromb.2025.124877","url":null,"abstract":"<div><div>Tryptophan-functionalized MOF-199 was synthesized via a simple solvothermal method and employed as a novel sorbent for the development of stir-bar sorptive extraction (SBSE) method. The extraction efficiency of the SBSE method was systematically investigated using warfarin and aspirin as model compounds. The extracted drugs were analyzed using high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Key parameters affecting SBSE, including stirring rate, desorption solvent, pH, extraction and desorption time, and salt concentration, were optimized, resulting in 800 rpm stirring rate, 5 min extraction, 1 min desorption, 11 % (<em>w</em>/<em>v</em>) salt concentration, 100.0 μL desorption solvent, and pH = 3.0 as optimal condition. Under the condition, the method exhibited excellent linearity (0.10–200.00 μg L<sup>−1</sup> for aspirin and 0.10–100.00 μg L<sup>−1</sup> for warfarin), low limits of detection (0.04 and 0.03 μg L<sup>−1</sup>) and limits of quantification (0.13 and 0.09 μg L<sup>−1</sup>), and satisfactory precision (%RSD = 4.40–7.60 % for aspirin and 5.10–6.50 % for warfarin). Enrichment factors (EFs) of 56.00 and 64.00 were achieved for aspirin and warfarin, respectively. The proposed SBSE-HPLC-UV method was successfully applied to biological samples, including plasma and urine, demonstrating high reproducibility, efficiency, and suitability for trace-level drug analysis. These results highlight the potential of tryptophan-functionalized MOF-199 as an effective sorbent for analytical applications in pharmaceutical and biological matrices. The method was further evaluated using the Blue Applicability Grade Index (BAGI), achieving a score of 82.5.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124877"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145663581","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

Refreshing the Aims and Scope of the Journal of Chromatography B 更新色谱杂志的目标和范围B。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-25 DOI: 10.1016/j.jchromb.2025.124865

David S. Hage, Huwei Liu, Georgios Theodoridis, Dimitrios Tsikas, Christina Virgilliou, Ian D. Wilson

引用次数: 0

Coupling complementary sample preparation methods and two-dimensional gas chromatography mass spectrometry with novel data workflows to the case of pollution in and from salmon aquaculture 耦合互补样品制备方法和二维气相色谱质谱与新的数据工作流程，以鲑鱼养殖污染的情况下

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-22 DOI: 10.1016/j.jchromb.2025.124860

Lisbet Sørensen , Mari Egeness Creese , Marie Ibrekk , Rikke Torvanger , Raymond Nepstad , Julie Metzger , Trond R. Størseth , Julia Farkas , Bjørn Henrik Hansen

Abstract

Navigating in the intersection between constantly increasing knowledge about ‘novel’ pollutants and their potential impact on the environment and human health, and answering the demand by consumers for evidence of seafood safety, is a challenge for the aquaculture industry and regulators both. Non-target and suspect analytical methods may offer part of the solution to this challenge. In the current study, we developed and tested a novel pipeline for non-target screening for the presence of organic pollutants using complementary extraction protocols and two-dimensional gas chromatography coupled with mass spectrometry. The pipeline was applied to identify organic pollutants in muscle samples of farmed Atlantic salmon (Salmo salar). Potential sources (intrinsic or environmental) were investigated through comparative analysis of feed pellets and local sediment samples. While no legacy contaminants were detected in either sample, a small suite of compounds of anthropogenic origin (preservatives, biocides, plasticizers and other plastic or chemical-industry-related compounds, as well as antioxidants and UV-stabilizers) was confidently detected, some of which may be candidates for future monitoring and mitigation actions.

摘要在不断增长的关于“新型”污染物及其对环境和人类健康的潜在影响的知识之间导航，以及回答消费者对海产品安全证据的需求，是水产养殖业和监管机构面临的挑战。非目标和可疑分析方法可能为这一挑战提供部分解决方案。在目前的研究中，我们开发并测试了一种新的管道，用于使用互补提取协议和二维气相色谱与质谱相结合的非目标筛选有机污染物的存在。该管道被用于鉴定养殖大西洋鲑鱼（Salmo salar）肌肉样本中的有机污染物。通过对饲料颗粒和当地沉积物样本的比较分析，调查了潜在的来源（内在或环境）。虽然在两个样品中都没有检测到遗留污染物，但有信心检测到一小部分人为来源的化合物（防腐剂、杀菌剂、增塑剂和其他与塑料或化学工业有关的化合物，以及抗氧化剂和紫外线稳定剂），其中一些可能是未来监测和缓解行动的候选物质。

{"title":"Coupling complementary sample preparation methods and two-dimensional gas chromatography mass spectrometry with novel data workflows to the case of pollution in and from salmon aquaculture","authors":"Lisbet Sørensen , Mari Egeness Creese , Marie Ibrekk , Rikke Torvanger , Raymond Nepstad , Julie Metzger , Trond R. Størseth , Julia Farkas , Bjørn Henrik Hansen","doi":"10.1016/j.jchromb.2025.124860","DOIUrl":"10.1016/j.jchromb.2025.124860","url":null,"abstract":"<div><div>Abstract</div><div>Navigating in the intersection between constantly increasing knowledge about ‘novel’ pollutants and their potential impact on the environment and human health, and answering the demand by consumers for evidence of seafood safety, is a challenge for the aquaculture industry and regulators both. Non-target and suspect analytical methods may offer part of the solution to this challenge. In the current study, we developed and tested a novel pipeline for non-target screening for the presence of organic pollutants using complementary extraction protocols and two-dimensional gas chromatography coupled with mass spectrometry. The pipeline was applied to identify organic pollutants in muscle samples of farmed Atlantic salmon (<em>Salmo salar</em>). Potential sources (intrinsic or environmental) were investigated through comparative analysis of feed pellets and local sediment samples. While no legacy contaminants were detected in either sample, a small suite of compounds of anthropogenic origin (preservatives, biocides, plasticizers and other plastic or chemical-industry-related compounds, as well as antioxidants and UV-stabilizers) was confidently detected, some of which may be candidates for future monitoring and mitigation actions.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124860"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145621744","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 a sea lamprey (Petromyzon marinus) pheromone antagonist in river water using ion pairing solid phase extraction coupled with liquid chromatography-tandem mass spectrometry 离子对固相萃取-液相色谱-串联质谱法定量测定河水中一种海鳗信息素拮抗剂。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-21 DOI: 10.1016/j.jchromb.2025.124866

Anne M. Scott, Sonam Tamrakar , Weiming Li

Pheromones mediate species-wide communication for many aquatic organisms, and the measurement of pheromones in natural waters is essential to understanding the environmental context of their function. However, chemical measurement of environmental pheromones and their antagonists is technically demanding and remains underdeveloped relative to assays for characterizing biological functions and application efficacy. In this study, we developed and validated an accurate and sensitive method to quantify a sea lamprey (Petromyzon marinus) pheromone and its antagonists. In this species, males release a multi-component sex pheromone containing 3-keto petromyzonol sulfate (3kPZS) that attracts females, while related compounds petromyzonol sulfate (PZS) and petromyzonol tetrasulfate (3sPZS) antagonize and disrupt female attraction. Developing methods to quantify 3sPZS in river water that contains pheromone is essential for understanding concentration-dependent effects of antagonists on invasive sea lamprey spawning. The target compound 3sPZS was extracted using triethylamine as an ion-pairing reagent during solid phase extraction followed by quantification using liquid chromatography-tandem mass spectrometry. The method showed a limit of detection of 0.1 ng/mL and limit of quantification of 0.5 ng/mL with linearity in the range of 10–1000 ng/mL. The intra- and inter-day accuracy, precision, recovery, and matrix effect of this method were evaluated. The method was applied to quantify 3sPZS, PZS, and 3kPZS in water sampled during field application in a river with sea lamprey and further evaluated for robustness by quantifying 3sPZS in 16 rivers across diverse environmental matrices. Our approach may be adapted to inform management strategies for detecting and mitigating invasive or imperiled aquatic species.

信息素介导了许多水生生物在物种范围内的交流，对自然水体中信息素的测量对于了解其功能的环境背景至关重要。然而，环境信息素及其拮抗剂的化学测量技术要求很高，相对于表征生物功能和应用效果的测定方法仍不发达。在本研究中，我们建立并验证了一种准确、灵敏的定量海七鳃鳗（Petromyzon marinus）信息素及其拮抗剂的方法。该物种雄性释放一种多组分性信息素，其中含有3-酮基石化苯二酚硫酸盐（3kPZS）吸引雌性，而相关化合物石化苯二酚硫酸盐（PZS）和石化苯二酚四硫酸酯（3sPZS）拮抗和破坏雌性的吸引力。研究含有信息素的河水中3sPZS的定量方法对于了解拮抗剂对入侵海七鳃鳗产卵的浓度依赖性作用至关重要。目的化合物3sPZS以三乙胺为离子配对试剂，固相萃取，液相色谱-串联质谱法定量。方法检出限为0.1 ng/mL，定量限为0.5 ng/mL，在10 ~ 1000 ng/mL范围内呈线性关系。评价了该方法的日内、日间准确度、精密度、回收率和基质效应。将该方法应用于一条有海七鳃鳗的河流的实地应用中，对采样水中的3sPZS、PZS和3kPZS进行量化，并通过对16条河流中不同环境矩阵的3sPZS进行量化，进一步评估其稳健性。我们的方法可以为检测和减轻入侵或濒危水生物种的管理策略提供信息。

{"title":"Quantification of a sea lamprey (Petromyzon marinus) pheromone antagonist in river water using ion pairing solid phase extraction coupled with liquid chromatography-tandem mass spectrometry","authors":"Anne M. Scott, Sonam Tamrakar , Weiming Li","doi":"10.1016/j.jchromb.2025.124866","DOIUrl":"10.1016/j.jchromb.2025.124866","url":null,"abstract":"<div><div>Pheromones mediate species-wide communication for many aquatic organisms, and the measurement of pheromones in natural waters is essential to understanding the environmental context of their function. However, chemical measurement of environmental pheromones and their antagonists is technically demanding and remains underdeveloped relative to assays for characterizing biological functions and application efficacy. In this study, we developed and validated an accurate and sensitive method to quantify a sea lamprey (<em>Petromyzon marinus</em>) pheromone and its antagonists. In this species, males release a multi-component sex pheromone containing 3-keto petromyzonol sulfate (3kPZS) that attracts females, while related compounds petromyzonol sulfate (PZS) and petromyzonol tetrasulfate (3sPZS) antagonize and disrupt female attraction. Developing methods to quantify 3sPZS in river water that contains pheromone is essential for understanding concentration-dependent effects of antagonists on invasive sea lamprey spawning. The target compound 3sPZS was extracted using triethylamine as an ion-pairing reagent during solid phase extraction followed by quantification using liquid chromatography-tandem mass spectrometry. The method showed a limit of detection of 0.1 ng/mL and limit of quantification of 0.5 ng/mL with linearity in the range of 10–1000 ng/mL. The intra- and inter-day accuracy, precision, recovery, and matrix effect of this method were evaluated. The method was applied to quantify 3sPZS, PZS, and 3kPZS in water sampled during field application in a river with sea lamprey and further evaluated for robustness by quantifying 3sPZS in 16 rivers across diverse environmental matrices. Our approach may be adapted to inform management strategies for detecting and mitigating invasive or imperiled aquatic species.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124866"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145592660","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 the simultaneous detection of urinary inflammatory biomarkers in a Flemish birth cohort 在佛兰德出生队列中同时检测尿液炎症生物标志物的LC-MS/MS方法的开发和验证。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-21 DOI: 10.1016/j.jchromb.2025.124867

Fatima den Ouden , Adam Cseresznye , Liesa Engelen , Elias Maris , Ellen De Paepe , Giulia Poma , Sebastian Proost , Arnau Vich i Vila , Lieselot Y. Hemeryck , Roger Pero-Gascon , Sarah De Saeger , Jeroen Raes , Lynn Vanhaecke , Tim S. Nawrot , Adrian Covaci

Chronic inflammation is a significant contributor to various diseases but its assessment via blood sampling presents challenges, particularly in children. The evaluation of urinary biomarkers, including 3-bromotyrosine (Bty), 3-chlorotyrosine (Cty) and leukotriene E4 (LTE4), offers a non-invasive alternative. This study presents the optimization and validation of a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of Bty, Cty and LTE4 in urine. Under optimized conditions, sample preparation was based on SPE using Oasis MAX cartridges, followed by LC-MS/MS analysis. Method performance was validated using the ICH 10 guidelines, resulting in satisfactory results for all analytes in terms of recovery, linearity, limits of quantification, precision and accuracy. Recovery rates ranged from 82 % to 97 %, while matrix effects were observed within the range of −11 % to 26 %. Linear range spanned from 0.08 to 20 ng/mL for the three analytes. Application to 332 urine samples from the ENVIRONAGE birth cohort (Belgium), comprising of children aged 4–11 years, revealed detection frequencies of 18 % for LTE4, 19 % for Cty and 50 % for Bty. Notably, creatinine-corrected Cty and LTE4 exhibited statistically significant Spearman correlations with established systemic inflammation markers. Specifically, Cty was positively correlated with absolute monocyte count (ρ = 0.53, p < 0.05), while LTE4 showed a positive correlation with relative eosinophil levels (ρ = 0.46, p < 0.05) and a negative correlation with the relative neutrophil levels (ρ = −0.56, p < 0.01). These results highlight the validated method as a valuable tool for investigating distinct inflammatory pathways in epidemiological settings and clinical research.

慢性炎症是各种疾病的重要因素，但通过血液采样进行评估存在挑战，特别是在儿童中。尿液生物标志物的评估，包括3-溴酪氨酸（Bty）、3-氯酪氨酸（Cty）和白三烯E4 (LTE4)，提供了一种非侵入性的替代方法。本研究优化并验证了液相色谱-串联质谱（LC-MS/MS）同时定量尿液中Bty、Cty和LTE4的方法。在优化后的条件下，采用Oasis MAX色谱筒进行固相萃取制备样品，然后进行LC-MS/MS分析。使用ICH 10指南验证了方法的性能，在回收率、线性度、定量限、精密度和准确度方面，所有分析物的结果都令人满意。回收率为82% ~ 97%，基质效应为- 11% ~ 26%。三种分析物的线性范围为0.08 ~ 20 ng/mL。应用来自ENVIRONAGE出生队列（比利时）的332份尿液样本，包括4-11岁的儿童，显示LTE4的检测频率为18%，Cty为19%，Bty为50%。值得注意的是，肌酐校正后的Cty和LTE4与已建立的全身性炎症标志物具有统计学上显著的Spearman相关性。具体而言，Cty与绝对单核细胞计数呈正相关(ρ = 0.53, p

{"title":"Development and validation of an LC-MS/MS method for the simultaneous detection of urinary inflammatory biomarkers in a Flemish birth cohort","authors":"Fatima den Ouden , Adam Cseresznye , Liesa Engelen , Elias Maris , Ellen De Paepe , Giulia Poma , Sebastian Proost , Arnau Vich i Vila , Lieselot Y. Hemeryck , Roger Pero-Gascon , Sarah De Saeger , Jeroen Raes , Lynn Vanhaecke , Tim S. Nawrot , Adrian Covaci","doi":"10.1016/j.jchromb.2025.124867","DOIUrl":"10.1016/j.jchromb.2025.124867","url":null,"abstract":"<div><div>Chronic inflammation is a significant contributor to various diseases but its assessment via blood sampling presents challenges, particularly in children. The evaluation of urinary biomarkers, including 3-bromotyrosine (Bty), 3-chlorotyrosine (Cty) and leukotriene E4 (LTE4), offers a non-invasive alternative. This study presents the optimization and validation of a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of Bty, Cty and LTE4 in urine. Under optimized conditions, sample preparation was based on SPE using Oasis MAX cartridges, followed by LC-MS/MS analysis. Method performance was validated using the ICH 10 guidelines, resulting in satisfactory results for all analytes in terms of recovery, linearity, limits of quantification, precision and accuracy. Recovery rates ranged from 82 % to 97 %, while matrix effects were observed within the range of −11 % to 26 %. Linear range spanned from 0.08 to 20 ng/mL for the three analytes. Application to 332 urine samples from the ENVIR<em>ON</em>AGE birth cohort (Belgium), comprising of children aged 4–11 years, revealed detection frequencies of 18 % for LTE4, 19 % for Cty and 50 % for Bty. Notably, creatinine-corrected Cty and LTE4 exhibited statistically significant Spearman correlations with established systemic inflammation markers. Specifically, Cty was positively correlated with absolute monocyte count (ρ = 0.53, <em>p</em> < 0.05), while LTE4 showed a positive correlation with relative eosinophil levels (ρ = 0.46, <em>p</em> < 0.05) and a negative correlation with the relative neutrophil levels (ρ = −0.56, <em>p</em> < 0.01). These results highlight the validated method as a valuable tool for investigating distinct inflammatory pathways in epidemiological settings and clinical research.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124867"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145608249","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

Optimizing the uptake of deuterated docosapentaenoic acid by salmonid liver cells using a uniform shell design and liquid chromatography triple-quadrupole mass spectrometry 采用均匀壳设计和液相色谱三重四极杆质谱法优化鲑鱼肝细胞对氘化二十五烯酸的吸收

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-21 DOI: 10.1016/j.jchromb.2025.124863

Pedro Araujo , Zhenxiao Zhuang , Maren Hoff Austgulen , Bjørg Kristine Hundal

Stable isotope-labelled fatty acids are valuable tracers for studying lipid metabolism in cell models. However, published methods rarely provide guidance on selecting the optimal concentration and incubation time to ensure accurate and reproducible measurements of cellular uptake and metabolism that reflect physiological conditions. This study systematically evaluated the uptake of deuterated docosapentaenoic acid (DPA-d₅) in Atlantic salmon (Salmo salar L.) liver cells using a uniform shell design methodology. Cultures were exposed to DPA-d₅ at concentrations ranging from 0 to 100 μM for 24, 48, or 72 h and the uptake was quantified in cell lysates by liquid chromatography–mass spectrometry. Results indicate that the concentration of DPA-d₅ has the strongest positive influence on signal intensity. Incubation time slightly reduces the signal, but when combined with higher concentration, it increases the uptake of DPA-d₅. Modelling of the data allowed selecting 60 μM DPA-d₅ and 48 h as the optimal culturing condition that provides a balance between achieving a strong signal and minimizing the risk of oversaturation or metabolic artifacts. This work provides a methodological foundation for future fatty acid tracer experiments in aquaculture research.

稳定的同位素标记脂肪酸是研究细胞脂质代谢模型的重要示踪剂。然而，已发表的方法很少对选择最佳浓度和孵育时间提供指导，以确保准确和可重复地测量反映生理条件的细胞摄取和代谢。本研究采用统一的壳设计方法，系统地评估了大西洋鲑鱼（Salmo salar L.）肝细胞对氘化二十五烯酸（DPA-d5）的吸收。培养物暴露于浓度从0到100 μM的DPA-d5中24、48或72小时，并通过液相色谱-质谱法定量细胞裂解物的摄取。结果表明，DPA-d₅的浓度对信号强度有最强的正向影响。孵育时间会略微降低信号，但当与更高浓度结合时，它会增加DPA-d₅的吸收。数据建模允许选择60 μM DPA-d5和48 h作为最佳培养条件，在获得强信号和最小化过饱和或代谢伪像风险之间提供平衡。本研究为今后脂肪酸示踪剂在水产养殖研究中的实验奠定了方法学基础。

{"title":"Optimizing the uptake of deuterated docosapentaenoic acid by salmonid liver cells using a uniform shell design and liquid chromatography triple-quadrupole mass spectrometry","authors":"Pedro Araujo , Zhenxiao Zhuang , Maren Hoff Austgulen , Bjørg Kristine Hundal","doi":"10.1016/j.jchromb.2025.124863","DOIUrl":"10.1016/j.jchromb.2025.124863","url":null,"abstract":"<div><div>Stable isotope-labelled fatty acids are valuable tracers for studying lipid metabolism in cell models. However, published methods rarely provide guidance on selecting the optimal concentration and incubation time to ensure accurate and reproducible measurements of cellular uptake and metabolism that reflect physiological conditions. This study systematically evaluated the uptake of deuterated docosapentaenoic acid (DPA-d<sub>5</sub>) in Atlantic salmon (<em>Salmo salar</em> L.) liver cells using a uniform shell design methodology. Cultures were exposed to DPA-d<sub>5</sub> at concentrations ranging from 0 to 100 μM for 24, 48, or 72 h and the uptake was quantified in cell lysates by liquid chromatography–mass spectrometry. Results indicate that the concentration of DPA-d₅ has the strongest positive influence on signal intensity. Incubation time slightly reduces the signal, but when combined with higher concentration, it increases the uptake of DPA-d₅. Modelling of the data allowed selecting 60 μM DPA-d<sub>5</sub> and 48 h as the optimal culturing condition that provides a balance between achieving a strong signal and minimizing the risk of oversaturation or metabolic artifacts. This work provides a methodological foundation for future fatty acid tracer experiments in aquaculture research.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124863"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145621747","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

Distinguishing native trisaccharides having differential monosaccharide composition and linkage using PGC-LC MS/MS 用PGC-LC质谱/质谱法鉴别具有不同单糖组成和连接的天然三糖。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-15 DOI: 10.1016/j.jchromb.2025.124849

Rose Mathew , P. Lijina , H.S. Varshitha , Gnanesh Kumar Belur Shivappa

Native glycosyl sucrose derivatives in plants represents primarily the trisaccharide isomers having different monosaccharides composition and linkage specificity. They can occur as complex mixtures wherein the separation and identification of individual trisaccharide becomes challenging. Herein, we employed porous graphitic carbon (PGC) liquid chromatography coupled to mass spectrometry to evaluate the elution order of major glycosyl sucrose trisaccharides and determined the structural feature through tandem mass spectrometry (MS/MS). Major trisaccharides comprised of galactosyl-, glucosyl- and fructosyl sucrose derivatives along with few reducing trisaccharides revealed distinct elution order. Furthermore, the application of this approach to profile the oligosaccharides in grape seeds showed the separation and identification of multiple native trisaccharides in the complex mixture that were hitherto unknown.

植物中天然糖基蔗糖衍生物主要是具有不同单糖组成和连锁特异性的三糖异构体。它们可以作为复杂的混合物出现，其中单个三糖的分离和鉴定变得具有挑战性。本研究采用多孔石墨碳（PGC）液相色谱-质谱联用技术对主要糖基蔗糖三糖的洗脱顺序进行评价，并通过串联质谱（MS/MS）测定其结构特征。由半乳糖、葡萄糖和果糖糖衍生物组成的主要三糖以及少数还原性三糖显示出不同的洗脱顺序。此外，将该方法应用于葡萄种子中低聚糖的分析表明，在复杂的混合物中分离和鉴定了多种迄今为止未知的天然三糖。

引用次数: 0

Rapid biocompatible solid phase microextraction: Nirogacestat protein binding in post dose human serum samples 快速生物相容性固相微萃取：硝加司他蛋白在给药后人血清样品中的结合。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-29 DOI: 10.1016/j.jchromb.2025.124874

Helen Patten , Rochelle Burke , Sohrab Habibi Goudarzi , Cassie Manning , Rex L. Williams Jr , Todd Baughman

Protein binding can influence the ability of a drug to permeate biologic membranes and can therefore be a limiting factor in the passage of drugs across a membrane. Most drugs must be unbound (free) to have a pharmacological effect. To quantitate free active drug in blood plasma, protein binding is typically assessed based on permeation techniques using devices such as a rapid equilibrium dialysis (RED) device. Caveats to this approach include the time to equilibration, which can introduce drug instability, and/or non-specific binding that confound accurate estimation of protein binding. Initial experiments with a RED device showed nirogacestat in clinical samples had non-specific binding in the buffer chamber which resulted in a low percent bound of 24.1 %. Clearly a different approach is needed to accurately characterize the protein binding of nirogacestat in clinical samples. For this reason, adsorption-based technologies, such as biocompatible solid phase microextraction (BioSPME), provide a potentially suitable alternative to permeation-based protein binding for highly bound drugs like nirogacestat.

BioSPME was used to measure protein binding for nirogacestat for both in vitro and clinical samples. A biocompatible sorbent material selectively extracts unbound analytes from a sample matrix as sample passes through the BioSPME cartridge, where the analyte is adsorbed onto the solid phase while the sample's base liquid passes through then eluted with a solvent. This approach allows for control of equilibration/incubation times and container types. The results show that BioSPME provides an accurate and reliable method for measuring protein binding in both in vitro and clinical samples.

Significance statement

BioSPME accurately measures the protein binding of nirogacestat in clinical serum samples and is an alternative to RED for measuring protein binding in vitro and in clinical samples.

蛋白质结合可以影响药物通过生物膜的能力，因此可以成为药物通过膜的限制因素。大多数药物必须是游离的才能产生药理作用。为了定量测定血浆中的游离活性药物，通常使用快速平衡透析（RED）装置等渗透技术来评估蛋白质结合。该方法的注意事项包括平衡时间，这可能会引入药物不稳定性和/或非特异性结合，从而混淆蛋白质结合的准确估计。用RED装置进行的初步实验表明，临床样品中的硝格司他在缓冲腔中具有非特异性结合，其结合率较低，为24.1%。显然，需要一种不同的方法来准确表征临床样品中硝格司他的蛋白质结合。出于这个原因，基于吸附的技术，如生物相容性固相微萃取（BioSPME），为像硝格司他这样的高结合药物提供了一种潜在的替代基于渗透的蛋白质结合的合适选择。BioSPME用于测定体外和临床样品中氮醋司他的蛋白结合。当样品通过BioSPME药筒时，生物相容性吸附剂材料选择性地从样品基质中提取未结合的分析物，其中分析物被吸附到固相上，而样品的基础液体通过，然后用溶剂洗脱。这种方法允许控制平衡/孵育时间和容器类型。结果表明，BioSPME在体外和临床样品中都提供了一种准确可靠的蛋白质结合测定方法。意义声明：BioSPME可准确测量临床血清样品中硝格司他的蛋白结合，是在体外和临床样品中测量蛋白结合的替代方法。

{"title":"Rapid biocompatible solid phase microextraction: Nirogacestat protein binding in post dose human serum samples","authors":"Helen Patten , Rochelle Burke , Sohrab Habibi Goudarzi , Cassie Manning , Rex L. Williams Jr , Todd Baughman","doi":"10.1016/j.jchromb.2025.124874","DOIUrl":"10.1016/j.jchromb.2025.124874","url":null,"abstract":"<div><div>Protein binding can influence the ability of a drug to permeate biologic membranes and can therefore be a limiting factor in the passage of drugs across a membrane. Most drugs must be unbound (free) to have a pharmacological effect. To quantitate free active drug in blood plasma, protein binding is typically assessed based on permeation techniques using devices such as a rapid equilibrium dialysis (RED) device. Caveats to this approach include the time to equilibration, which can introduce drug instability, and/or non-specific binding that confound accurate estimation of protein binding. Initial experiments with a RED device showed nirogacestat in clinical samples had non-specific binding in the buffer chamber which resulted in a low percent bound of 24.1 %. Clearly a different approach is needed to accurately characterize the protein binding of nirogacestat in clinical samples. For this reason, adsorption-based technologies, such as biocompatible solid phase microextraction (BioSPME), provide a potentially suitable alternative to permeation-based protein binding for highly bound drugs like nirogacestat.</div><div>BioSPME was used to measure protein binding for nirogacestat for both <em>in vitro</em> and clinical samples. A biocompatible sorbent material selectively extracts unbound analytes from a sample matrix as sample passes through the BioSPME cartridge, where the analyte is adsorbed onto the solid phase while the sample's base liquid passes through then eluted with a solvent. This approach allows for control of equilibration/incubation times and container types. The results show that BioSPME provides an accurate and reliable method for measuring protein binding in both <em>in vitro</em> and clinical samples.</div></div><div><h3>Significance statement</h3><div>BioSPME accurately measures the protein binding of nirogacestat in clinical serum samples and is an alternative to RED for measuring protein binding <em>in vitro</em> and in clinical samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124874"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145688850","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

Hierarchical C-Fe2O3@MnO2 nanostructured sorbent; application in dispersive-μ-solid phase extraction of antifungal drugs 分级C-Fe2O3@MnO2纳米结构吸附剂；分散μ-固相萃取法在抗真菌药物中的应用。

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-19 DOI: 10.1016/j.jchromb.2025.124858

Hanieh Riazi Bonab , Amir Abbas Matin , Mustafa Soylak

In the current work, a hierarchical nanocomposite based on MnO₂ nanosheets attached to the C-Fe₂O₃ substrate (C-Fe₂O₃@MnO₂) was introduced as a novel and efficient dispersive-μ-solid phase extraction sorbent. The well-prepared nanocomposite with unique morphology leading to higher surface area, high porosity, and excellent adsorptive capacity was used for preconcentration of antifungal drugs (ketoconazole, clotrimazole, and miconazole) from plasma and wastewater samples before analysis using high-performance liquid chromatography (HPLC-UV). The synthesized nanosorbent was characterized using XRD, FTIR, FE-SEM, BET/BJH, and EDX analysis. In the optimal condition, the limit of detection (LODs) and the limit of quantification (LOQs) were acquired as 1.5, 5.0 μg L⁻¹ in the linear range of 5–500 μg L⁻¹ in plasma samples and 0.3, 1.0 μg L⁻¹ in the linear range of 1–150 μg L⁻¹ in wastewater samples for all analytes. Furthermore, the relative standard deviations (RSD%) for the repeatability of the sorbent synthesis method and reusability of one sorbent were found to be 0.92, 1.23, 1.32 % and 2.43, 3.15, 4.28 % for ketoconazole, clotrimazole, and miconazole, respectively.

本文介绍了一种新型、高效的分散μ固相萃取吸附剂——MnO2纳米片与C-Fe2O3衬底（C-Fe2O3@MnO2）的层次化纳米复合材料。制备的纳米复合材料具有独特的形貌，具有更高的表面积、高孔隙率和优异的吸附能力，用于预富集血浆和废水样品中的抗真菌药物（酮康唑、克霉唑和咪康唑），然后使用高效液相色谱（HPLC-UV）进行分析。采用XRD、FTIR、FE-SEM、BET/BJH和EDX对合成的纳米吸附剂进行了表征。在最佳条件下，血浆样品在5 ~ 500 μ L-1线性范围内的检出限（lod）和定量限（loq）分别为1.5、5.0 μ L-1，废水样品在1 ~ 150 μ L-1线性范围内的定量限（loq）分别为0.3、1.0 μ L-1。酮康唑、克霉唑和咪康唑的重复性和可重复使用性的相对标准偏差（RSD%）分别为0.92、1.23、1.32%和2.43、3.15、4.28%。

{"title":"Hierarchical C-Fe2O3@MnO2 nanostructured sorbent; application in dispersive-μ-solid phase extraction of antifungal drugs","authors":"Hanieh Riazi Bonab , Amir Abbas Matin , Mustafa Soylak","doi":"10.1016/j.jchromb.2025.124858","DOIUrl":"10.1016/j.jchromb.2025.124858","url":null,"abstract":"<div><div>In the current work, a hierarchical nanocomposite based on MnO<sub>2</sub> nanosheets attached to the C-Fe<sub>2</sub>O<sub>3</sub> substrate (C-Fe<sub>2</sub>O<sub>3</sub>@MnO<sub>2</sub>) was introduced as a novel and efficient dispersive-μ-solid phase extraction sorbent. The well-prepared nanocomposite with unique morphology leading to higher surface area, high porosity, and excellent adsorptive capacity was used for preconcentration of antifungal drugs (ketoconazole, clotrimazole, and miconazole) from plasma and wastewater samples before analysis using high-performance liquid chromatography (HPLC-UV). The synthesized nanosorbent was characterized using XRD, FTIR, FE-SEM, BET/BJH, and EDX analysis. In the optimal condition, the limit of detection (LODs) and the limit of quantification (LOQs) were acquired as 1.5, 5.0 μg L<sup>−1</sup> in the linear range of 5–500 μg L<sup>−1</sup> in plasma samples and 0.3, 1.0 μg L<sup>−1</sup> in the linear range of 1–150 μg L<sup>−1</sup> in wastewater samples for all analytes. Furthermore, the relative standard deviations (RSD%) for the repeatability of the sorbent synthesis method and reusability of one sorbent were found to be 0.92, 1.23, 1.32 % and 2.43, 3.15, 4.28 % for ketoconazole, clotrimazole, and miconazole, respectively.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124858"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145608322","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

Identification of potential TMPRSS2 inhibitors via high-throughput screening based on oriented immobilized cell membrane chromatography technology 基于定向固定化细胞膜色谱技术的高通量筛选鉴定潜在TMPRSS2抑制剂

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2026-01-15 Epub Date: 2025-11-19 DOI: 10.1016/j.jchromb.2025.124861

Siqi Wang , Min Si , Qihuan Liao , Yifei Li , Wenyu Yang , Huaizhen He , Cheng Wang

The transmembrane protease serine 2 (TMPRSS2) plays a crucial role in the cellular entry of coronaviruses, making the search for its inhibitors pertinent for developing novel antiviral drugs. Cell membrane chromatography (CMC) is a novel methodology that immobilizes membrane receptors on silica gel, utilizing chromatographic techniques to discover new drugs. To enhance the accuracy of this method, this study employed styrene-maleic acid (SMA) copolymers for protein extraction His-tag for protein immobilization, which would minimize alterations to the biological structure of TMPRSS2. Methodological validation demonstrated that this model offers improved reproducibility and longer column lifespan compared to traditional CMC columns, alongside superior screening performance. Utilizing this model, a screening campaign was conducted against a commercial small molecule library containing 3010 compounds. Preliminary activity validation revealed that the screened famotidine and TS0665 effectively inhibited pseudovirus infection of cells. These findings provide an experimental foundation for the subsequent development of antiviral therapeutics.

跨膜蛋白酶丝氨酸2 （TMPRSS2）在冠状病毒进入细胞中起着至关重要的作用，因此寻找其抑制剂与开发新型抗病毒药物有关。细胞膜色谱（CMC）是一种将膜受体固定在硅胶上，利用色谱技术发现新药的新方法。为了提高该方法的准确性，本研究采用苯乙烯-马来酸（SMA）共聚物进行蛋白质提取，His-tag用于蛋白质固定，从而最大限度地减少对TMPRSS2生物结构的改变。方法学验证表明，与传统CMC色谱柱相比，该模型具有更好的可重复性和更长的柱寿命，同时具有优越的筛选性能。利用该模型，对含有3010种化合物的商业小分子文库进行了筛选。初步活性验证表明，筛选得到的法莫替丁和TS0665均能有效抑制细胞的假病毒感染。这些发现为后续抗病毒疗法的发展提供了实验基础。

{"title":"Identification of potential TMPRSS2 inhibitors via high-throughput screening based on oriented immobilized cell membrane chromatography technology","authors":"Siqi Wang , Min Si , Qihuan Liao , Yifei Li , Wenyu Yang , Huaizhen He , Cheng Wang","doi":"10.1016/j.jchromb.2025.124861","DOIUrl":"10.1016/j.jchromb.2025.124861","url":null,"abstract":"<div><div>The transmembrane protease serine 2 (TMPRSS2) plays a crucial role in the cellular entry of coronaviruses, making the search for its inhibitors pertinent for developing novel antiviral drugs. Cell membrane chromatography (CMC) is a novel methodology that immobilizes membrane receptors on silica gel, utilizing chromatographic techniques to discover new drugs. To enhance the accuracy of this method, this study employed styrene-maleic acid (SMA) copolymers for protein extraction His-tag for protein immobilization, which would minimize alterations to the biological structure of TMPRSS2. Methodological validation demonstrated that this model offers improved reproducibility and longer column lifespan compared to traditional CMC columns, alongside superior screening performance. Utilizing this model, a screening campaign was conducted against a commercial small molecule library containing 3010 compounds. Preliminary activity validation revealed that the screened famotidine and TS0665 effectively inhibited pseudovirus infection of cells. These findings provide an experimental foundation for the subsequent development of antiviral therapeutics.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1269 ","pages":"Article 124861"},"PeriodicalIF":2.8,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145546402","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