Journal of separation science最新文献

{"title":"Counter-Current Chromatography Separation of Arenobufagin Glycosylation Products With Improved Safety and Anti-Inflammatory Activity","authors":"Feilong Zhao,&nbsp;Xinxin Liu,&nbsp;Fangfang He,&nbsp;Yujie Lei,&nbsp;Qinglan Li,&nbsp;Qiqi Wang,&nbsp;Denglang Zou","doi":"10.1002/jssc.70544","DOIUrl":"https://doi.org/10.1002/jssc.70544","url":null,"abstract":"<div>\u0000 \u0000 <p>Arenobufagin, a typical bufadienolide from toad venom, exhibits excellent anti-inflammatory activity; however, its inherent toxicity severely limits its further application. To improve its safety profile, this study employed glycosylation for the structural modification of arenobufagin. Given the complexity of the reaction matrix, counter-current chromatography (CCC) was selected for the efficient separation of the glycosylated products. First, response surface methodology was employed to optimize the glycosylation reaction conditions, which significantly enhanced the conversion rate. The glycosylation products were successfully separated using a solvent system composed of dichloromethane/methanol/water (8:4:8, v/v/v). From a 550 mg crude sample, 14.6 mg of arenobufagin-3-O-β-D-glucosyl (1→2)-β-D-glucoside (Arenobufagin-2G), 80.3 mg of arenobufagin-3-O-β-D-glucoside, and 17.5 mg of the unreacted arenobufagin substrate were obtained. Biological evaluation revealed that arenobufagin conjugated with two sugar moieties achieved a favorable balance between safety and anti-inflammatory efficacy. Mechanistically, Arenobufagin-2G suppressed inflammatory responses in Tohoku Hospital pediatrics-1-derived macrophages and attenuated lipopolysaccharide-induced nucleotide-binding domain, leucine-rich repeat, and pyrin domain-containing protein 3 inflammasome activation. This study not only demonstrates that CCC is a powerful strategy for separating complex glycosylation products but also lays the foundation for the future research and development of safe arenobufagin-based therapeutics.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149072619","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Counter-Current Chromatography Separation of Arenobufagin Glycosylation Products With Improved Safety and Anti-Inflammatory Activity","authors":"Feilong Zhao,&nbsp;Xinxin Liu,&nbsp;Fangfang He,&nbsp;Yujie Lei,&nbsp;Qinglan Li,&nbsp;Qiqi Wang,&nbsp;Denglang Zou","doi":"10.1002/jssc.70544","DOIUrl":"https://doi.org/10.1002/jssc.70544","url":null,"abstract":"<div>\u0000 \u0000 <p>Arenobufagin, a typical bufadienolide from toad venom, exhibits excellent anti-inflammatory activity; however, its inherent toxicity severely limits its further application. To improve its safety profile, this study employed glycosylation for the structural modification of arenobufagin. Given the complexity of the reaction matrix, counter-current chromatography (CCC) was selected for the efficient separation of the glycosylated products. First, response surface methodology was employed to optimize the glycosylation reaction conditions, which significantly enhanced the conversion rate. The glycosylation products were successfully separated using a solvent system composed of dichloromethane/methanol/water (8:4:8, v/v/v). From a 550 mg crude sample, 14.6 mg of arenobufagin-3-O-β-D-glucosyl (1→2)-β-D-glucoside (Arenobufagin-2G), 80.3 mg of arenobufagin-3-O-β-D-glucoside, and 17.5 mg of the unreacted arenobufagin substrate were obtained. Biological evaluation revealed that arenobufagin conjugated with two sugar moieties achieved a favorable balance between safety and anti-inflammatory efficacy. Mechanistically, Arenobufagin-2G suppressed inflammatory responses in Tohoku Hospital pediatrics-1-derived macrophages and attenuated lipopolysaccharide-induced nucleotide-binding domain, leucine-rich repeat, and pyrin domain-containing protein 3 inflammasome activation. This study not only demonstrates that CCC is a powerful strategy for separating complex glycosylation products but also lays the foundation for the future research and development of safe arenobufagin-based therapeutics.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149072575","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Room-Temperature Synthesis of Anionic Covalent Organic Framework Monolithic Materials for Efficient Capturing of Berberine Hydrochloride","authors":"Xingyun Zhao,&nbsp;Zhenwei Zhang,&nbsp;Junjie Zhang,&nbsp;Zhiqin Qin,&nbsp;Lijuan Yan,&nbsp;Xiaojing Yang,&nbsp;Weidong Wu,&nbsp;Liyun Zhang,&nbsp;Rongfang Wu","doi":"10.1002/jssc.70514","DOIUrl":"10.1002/jssc.70514","url":null,"abstract":"<div>\u0000 \u0000 <p>An anionic covalent organic framework (COF) was constructed using 2,5-diaminobenzenesulfonic acid as an ionic building unit. The incorporation of sulfonate functionalities endows the framework with permanent anionic sites, thereby enabling selective ion-exchange interactions with cationic species. The adsorption performance toward berberine hydrochloride (BBH) was systematically investigated by optimizing pH, ionic strength, adsorbent dosage, extraction time, and elution conditions. Rapid adsorption equilibrium was achieved within 10 min, and the kinetic data were well described by a pseudo-second-order model, indicating a chemisorption-dominated process. Under optimal conditions (pH 11, 303 K), the maximum adsorption capacity reached 1082.4 mg g⁻¹. The material maintained high adsorption efficiency in the presence of competing cations, demonstrating pronounced selectivity arising from electrostatic interactions. Moreover, it retained over 90% of its initial adsorption capacity after five adsorption–desorption cycles, confirming its structural stability and recyclability. These results highlight the effectiveness of introducing ionic functionalities into COF architectures to achieve high-capacity and selective adsorption of alkaloid compounds, providing a viable platform for the separation and analysis of BBH in complex herbal matrices. The design and synthesis of novel COF porous adsorption materials will play a crucial role in the separation and analysis of natural products.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 9","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148963413","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Preparation of Gemini-Functionalized Cellulose Paper Sorptive Phases for Enrichment of Non-Steroidal Anti-Inflammatory Drugs in Water","authors":"Shuai Luo,&nbsp;Rui Liu,&nbsp;Zhong-Hui Sun,&nbsp;Zhou-Yang Xiang,&nbsp;Hua-Jie Lai,&nbsp;Bo Liu","doi":"10.1002/jssc.70537","DOIUrl":"10.1002/jssc.70537","url":null,"abstract":"<div>\u0000 \u0000 <p>Cationic cellulose paper is a promising adsorbent for acidic compounds in water. However, cellulose modified with glycidyl trimethyl ammonium chloride (EPTAC) often exhibits compromised structural integrity and readily disperses in water. In this study, a Gemini quaternary ammonium salt (Gemini-QAS) was synthesized via nucleophilic substitution of <i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethyl-1,6-hexanediamine with epichlorohydrin and subsequently used for the etherification of cellulose paper. Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and zeta potential analyses confirmed the successful incorporation of the Gemini-QAS onto the cellulose substrate. Tensile testing demonstrated that the Gemini-modified cellulose paper (GCP) exhibited enhanced mechanical strength in both dry (25.16 MPa) and wet (1.54 KN/m) states, and the wet tensile strength ratio was 0.29, whereas EPTAC-modified cellulose paper showed decreased wet tensile strength (0.51 KN/m) and ratio (0.16). Batch experiments demonstrated that the optimal adsorption and desorption conditions for GCP on 12 weakly acidic non-steroidal anti-inflammatory drugs (NSAIDs) were pH 7.0, an adsorption time of 30 min, and an eluent of 2% formic acid-methanol. Then, these 12 NSAIDs were extracted by GCP from real water samples and quantified by high-performance liquid chromatography-tandem mass spectrometry. The analytical method achieved limits of detection ranging from 0.02 to 0.64 µg/L and limits of quantification between 0.07 and 2.11 µg/L. Precision, expressed as intra-day relative standard deviation (RSD), remained below 10%, and inter-day RSD below 12%. The relative recoveries ranged from 71% to 102% at spiking levels of 10 and 50 µg/L, while recoveries at 1 µg/L ranged from 65.1% to 89.7% due to more pronounced matrix effects. This work successfully resolves the poor aqueous stability and fiber dispersion issues of EPTAC-modified cellulose, providing a green, low-cost, and robust paper-based sorptive phase for trace NSAID monitoring in environmental water, which aligns with the principles of sustainable analytical chemistry.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 9","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148963463","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Prediction of Elution Profiles in Countercurrent Chromatography With a Linear Loss of Stationary Phase","authors":"Felix Rüttler,&nbsp;Rosalie Ormos,&nbsp;Walter Vetter","doi":"10.1002/jssc.70526","DOIUrl":"10.1002/jssc.70526","url":null,"abstract":"<p>Countercurrent chromatography (CCC) is a liquid-liquid separation method that is predominantly used for the preparative isolation of natural products. Key indicators for the development of CCC methods are the partition coefficient (<i>K</i> value) between the two liquid phases and the properties of the chosen biphasic solvent system. Based on this information, it is possible to predict elution volumes and peak widths with the probabilistic model for immiscible separations and extractions (ProMISE). However, a common challenge in reliably predicting CCC elution profiles is a persistent loss of stationary phase (i.e., bleeding), which leads to a decrease in the percentile share of stationary phase (<i>S_f</i> value) in the column as the separation progresses. In this study, two carotenoids were isolated and used as test compounds to investigate the effect of bleeding with the <i>n</i>-hexane/benzotrifluoride/acetonitrile (20:7:13, <i>v</i>/<i>v</i>/<i>v</i>) solvent system. After showing that the stationary phase bleeding rate was linear (and not exponential), experiments were carried out both in head-to-tail and in tail-to-head mode. Next, a simple calibration method was developed to predict elution volumes and peak widths with the ProMISE2 software in CCC separations with linear bleeding. Finally, based on the collected data, a method was developed to accurately predict the elution volume and peak width during a (long) CCC run, particularly for analytes with comparatively high elution volumes.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 9","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13572847/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148963398","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Enantiomers of Deschloroketamine and Its Metabolites in Wistar Rat Brains","authors":"Natalie Paškanová,&nbsp;Vendulka Hrubá,&nbsp;Peter Frühauf,&nbsp;Bronislav Jurásek,&nbsp;Martin Kuchař,&nbsp;Pavel Řezanka,&nbsp;Michal Kohout","doi":"10.1002/jssc.70503","DOIUrl":"10.1002/jssc.70503","url":null,"abstract":"<p>Deschloroketamine (DXE) is a dissociative new psychoactive substance whose enantiomers and metabolites may exhibit distinct pharmacological and toxicological profiles. Reliable analytical methods enabling the chiral determination of DXE and its metabolites in biological matrices are thus essential. In this study, we evaluated supercritical fluid chromatography coupled to tandem mass spectrometry (SFC‑MS/MS) and capillary zone electrophoresis with ultraviolet detection (CZE‑UV) for the enantioselective analysis of DXE and its major metabolites in rat brain tissue. SFC using polysaccharide‑based chiral stationary phases provided baseline separation of the hydroxylated and demethylated metabolites, but severe peak distortion of DXE enantiomers prevented their quantification. Therefore, quantitative analysis was performed by CZE employing carboxymethyl‑β‑cyclodextrin as a chiral selector and a high‑sensitivity Z‑shaped detection cell. Analysis of brain tissue samples obtained following high-dose administration revealed near equimolar concentrations of the DXE enantiomers and a higher concentration of (<i>R</i>)-norDXE relative to (<i>S</i>)-norDXE. In this particular case, the combined use of SFC‑MS/MS and CZE‑UV provided a practical workflow for the chiral profiling of DXE and its metabolites in complex biological matrices.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 9","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13572844/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148963400","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Systematic Evaluation of Partition-Dominated Retention in Hydrophilic Interaction Liquid Chromatography (HILIC) Under Varying Aqueous Components of the Mobile Phase: Revisiting the HILIC Column Test Scheme","authors":"Tomoaki Shimpo,&nbsp;Tohru Ikegami","doi":"10.1002/jssc.70520","DOIUrl":"10.1002/jssc.70520","url":null,"abstract":"<div>\u0000 \u0000 <p>The robustness of a test for characterizing hydrophilic interaction liquid chromatography (HILIC) columns against variations in aqueous mobile-phase composition was evaluated using mobile phases of acetonitrile/aqueous mixture (9:1, v/v) in the pH range of 3.6–6.8 of the aqueous part. Ten columns (commercially available and home-made columns) were examined under five mobile phases differing in anion species (formate or acetate), NH₄⁺ concentration and salt concentration. The specific hydrophilicity of the columns was assessed via the retention factor of uridine (<i>k</i>(U)), and the relative retention characteristics (i.e., retention selectivity: <i>α</i>) were evaluated using structure-related probe pairs. The <i>k</i>(U)-values exhibited low variability under low-salt conditions (20 mM in the aqueous part; CVs = 0.01–0.08), but higher variability under high-salt conditions (100 mM in the aqueous part; CVs = 0.03–0.18). Under comparable pH conditions (ammonium formate at pH 4.5 vs. ammonium acetate at pH 4.7), <i>k</i>(U)-values were consistently higher in the former, indicating that differences in NH₄⁺ concentration affect hydration at the stationary-phase interface and thereby influence retention. This suggests that <i>k</i>(U), commonly used as an indicator of hydrophilic retention, can be affected significantly by partition interactions that are controlled by ionic concentration rather than the pH value of the mobile phase. In contrast, the characteristic <i>α</i>-values primarily associated with solute retention via partitioning exhibited high robustness (CVs ≤ 0.03). Notably, <i>α</i>(<i>k</i>(U)/<i>k</i>(2′-deoxyuridine)) values correlated with the estimated phase ratio, suggesting that it reflects the effective volume of the hydrated layer on the surface of the packing materials. Furthermore, the relationships between <i>α</i>(<i>k</i>(1-β-D-arabinofuranosyl uracil)/<i>k</i>(U)) and <i>α</i>(<i>k</i>(vidarabine)/<i>k</i>(adenosine)) indicated that nucleobase‑dependent interactions contribute significantly to stationary‑phase retention. Overall, these results demonstrate that each <i>k</i>(U) and <i>α</i>, particularly those associated with partition-dominated retention, exhibit generally high robustness within this test framework and provide a basis for more robust and transferable HILIC column characterization.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 9","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148962946","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Selective Screening of Dual-Target Bioactive Constituents From Shaoqitongfei Formula Against Chronic Obstructive Pulmonary Disease by Receptor Chromatography","authors":"Yunshan Wang,&nbsp;Yangyang Zhang,&nbsp;Kexin Li,&nbsp;Zihu Wang,&nbsp;Jia Wang,&nbsp;Qian Li","doi":"10.1002/jssc.70535","DOIUrl":"https://doi.org/10.1002/jssc.70535","url":null,"abstract":"<div>\u0000 \u0000 <p>Current mainstream treatment of chronic obstructive pulmonary disease (COPD) relies largely on long-acting β₂-adrenergic receptor (β₂AR) agonists and muscarinic M₃ receptor (M₃R) antagonists, yet residual inflammation and variable treatment responses persist. Developing therapeutics from multicomponent herbal medicines is an effective drug development approach but is constrained by the difficulty of linking individual constituents to pharmacologically relevant targets and in vivo efficacy. This study established an integrated discovery workflow combining whole-formula efficacy testing, receptor-affinity chromatography, mass spectrometry (MS), and in vivo validation of candidate combinations. We applied this workflow to the Shaoqitongfei formula (SQTF), an investigator-developed three-herb prescription evaluated for ameliorating COPD, and selected the β₂AR and M₃R as clinically relevant bronchodilator targets. In porcine pancreatic elastase/lipopolysaccharide (LPS)-induced COPD mice, SQTF improved respiratory parameters, attenuated lung injury, and reduced inflammatory cytokine levels in serum and bronchoalveolar lavage fluid. Affinity columns containing immobilized β₂AR and M₃R stationary phases were utilized to screen the receptor-targeting components in formula extract. High-performance liquid chromatography-tandem MS analysis tentatively annotated albiflorin and kaempferol in the extract retained by both columns. In rats exposed to cigarette smoke and LPS, co-administration of albiflorin and kaempferol reproduced several of the pulmonary and anti-inflammatory effects of SQTF and shifted protein-expression patterns associated with signaling proteins to those observed in controls. Taken together, these findings establish a receptor-guided workflow for selecting pharmacologically relevant constituent combinations from complex herbal medicines and provide an analytical basis for the further development of SQTF-derived therapies for COPD.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 9","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148943321","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Selective Screening of Dual-Target Bioactive Constituents From Shaoqitongfei Formula Against Chronic Obstructive Pulmonary Disease by Receptor Chromatography","authors":"Yunshan Wang,&nbsp;Yangyang Zhang,&nbsp;Kexin Li,&nbsp;Zihu Wang,&nbsp;Jia Wang,&nbsp;Qian Li","doi":"10.1002/jssc.70535","DOIUrl":"https://doi.org/10.1002/jssc.70535","url":null,"abstract":"<div>\u0000 \u0000 <p>Current mainstream treatment of chronic obstructive pulmonary disease (COPD) relies largely on long-acting β₂-adrenergic receptor (β₂AR) agonists and muscarinic M₃ receptor (M₃R) antagonists, yet residual inflammation and variable treatment responses persist. Developing therapeutics from multicomponent herbal medicines is an effective drug development approach but is constrained by the difficulty of linking individual constituents to pharmacologically relevant targets and in vivo efficacy. This study established an integrated discovery workflow combining whole-formula efficacy testing, receptor-affinity chromatography, mass spectrometry (MS), and in vivo validation of candidate combinations. We applied this workflow to the Shaoqitongfei formula (SQTF), an investigator-developed three-herb prescription evaluated for ameliorating COPD, and selected the β₂AR and M₃R as clinically relevant bronchodilator targets. In porcine pancreatic elastase/lipopolysaccharide (LPS)-induced COPD mice, SQTF improved respiratory parameters, attenuated lung injury, and reduced inflammatory cytokine levels in serum and bronchoalveolar lavage fluid. Affinity columns containing immobilized β₂AR and M₃R stationary phases were utilized to screen the receptor-targeting components in formula extract. High-performance liquid chromatography-tandem MS analysis tentatively annotated albiflorin and kaempferol in the extract retained by both columns. In rats exposed to cigarette smoke and LPS, co-administration of albiflorin and kaempferol reproduced several of the pulmonary and anti-inflammatory effects of SQTF and shifted protein-expression patterns associated with signaling proteins to those observed in controls. Taken together, these findings establish a receptor-guided workflow for selecting pharmacologically relevant constituent combinations from complex herbal medicines and provide an analytical basis for the further development of SQTF-derived therapies for COPD.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 9","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148943235","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Bipyridine-functionalized Covalent Organic Framework as a Reusable Adsorbent for Trace BTEX Detection in Water Samples","authors":"Zhiqun Xu,&nbsp;Fangpei Ma,&nbsp;Tianju Chen,&nbsp;Bo Hou,&nbsp;Quan Cheng,&nbsp;Pingping Fan,&nbsp;Yueping Zheng,&nbsp;Lan Fang,&nbsp;Jianhua Wang","doi":"10.1002/jssc.70529","DOIUrl":"10.1002/jssc.70529","url":null,"abstract":"<div>\u0000 \u0000 <p>Benzene, toluene, ethylbenzene, and xylenes (BTEX) are hazardous volatile organic compounds frequently detected in environmental waters, posing serious risks to human health and ecosystems. Therefore, sensitive and reliable analytical methods for trace BTEX monitoring are urgently needed. In this work, a novel imine-linked covalent organic framework (TAPB-Bpy) containing bipyridine units was synthesized via Schiff-base reaction and applied as a dispersive solid-phase extraction (d-SPE) adsorbent for the preconcentration of BTEX coupled with gas chromatography-flame ionization detection (GC-FID). Benefiting from its highly ordered porous structure, good thermal stability and abundant π-electron-rich sites, TAPB-Bpy exerts strong π-π stacking and weak C-H···N hydrogen bonding interactions with BTEX molecules, as verified by XPS analysis. Under optimized conditions, the method achieved a linear range of 0.003–10 µg L⁻¹, limits of detection (LODs) of 0.001 µg L⁻¹ for all four analytes, and good reproducibility with relative standard deviations (RSDs) below 8.1%. The adsorbent retained stable extraction efficiency after at least 30 reuse cycles, showing favorable cost-effectiveness. Compared with recently reported SPE/SPME methods for BTEX determination, our approach provides 2-10-fold lower LODs, a broader linear range, and superior reusability. When applied to real water samples including tap water, river water, rainwater, and industrial wastewater, satisfactory recoveries ranging from 90.9% to 109.6% were obtained, with RSDs between 1.0% and 9.0%. These results indicate that TAPB-Bpy is a promising d-SPE adsorbent for trace BTEX analysis in complex environmental matrices.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 9","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148930198","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}