Pub Date : 2026-03-29Epub Date: 2026-01-28DOI: 10.1016/j.chroma.2026.466755
Fei Wang , Yuting Ren , Ran Song , Guiru Chen , Hongyu Wang , Luying Wang , Jing Liu , Jiandu Lei
Developing sustainable and efficient separation technologies is crucial for achieving a green transformation in the bioprocessing industry. This study proposes an innovative chromatographic material that utilizes abundant pine wood as raw material. It employs a dextran grafting strategy to functionalize the substrate, resulting in the preparation of high-capacity anion-exchange monolithic columns. This method serves as a robust sustainability strategy, converting low-value biomass into high-value separation media. The optimized monolithic material exhibits a static adsorption capacity of 122.1 mg g-1 for bovine serum albumin and a dynamic capacity of over 97 mg g-1. Leveraging the natural convective channels within wood, the material achieves rapid binding kinetics and exhibits excellent column permeability of 1.12 × 10-10 m2. Its exceptional reusability (over 100 cycles) and long-term stability further demonstrate its practicality and economic viability. We validated its practical application value by successfully purifying target proteins from complex mixtures. This work integrates fundamental material innovation with scalable bioprocessing technology to provide a sustainable, high-performance, and cost-effective platform for purifying proteins and other high-value bioproducts.
{"title":"Utilization of dextran grafting to prepare high-performance wood monolith for efficient bioseparation","authors":"Fei Wang , Yuting Ren , Ran Song , Guiru Chen , Hongyu Wang , Luying Wang , Jing Liu , Jiandu Lei","doi":"10.1016/j.chroma.2026.466755","DOIUrl":"10.1016/j.chroma.2026.466755","url":null,"abstract":"<div><div>Developing sustainable and efficient separation technologies is crucial for achieving a green transformation in the bioprocessing industry. This study proposes an innovative chromatographic material that utilizes abundant pine wood as raw material. It employs a dextran grafting strategy to functionalize the substrate, resulting in the preparation of high-capacity anion-exchange monolithic columns. This method serves as a robust sustainability strategy, converting low-value biomass into high-value separation media. The optimized monolithic material exhibits a static adsorption capacity of 122.1 mg g<sup>-1</sup> for bovine serum albumin and a dynamic capacity of over 97 mg g<sup>-1</sup>. Leveraging the natural convective channels within wood, the material achieves rapid binding kinetics and exhibits excellent column permeability of 1.12 × 10<sup>-10</sup> m<sup>2</sup>. Its exceptional reusability (over 100 cycles) and long-term stability further demonstrate its practicality and economic viability. We validated its practical application value by successfully purifying target proteins from complex mixtures. This work integrates fundamental material innovation with scalable bioprocessing technology to provide a sustainable, high-performance, and cost-effective platform for purifying proteins and other high-value bioproducts.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466755"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146111747","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The development of chromatographic stationary phases remains a persistent focus of scientific inquiry, as their functions and properties directly determine separation efficiency and application scope. Although hydrogel-based stationary phases exhibit prominent advantages such as customizable functionalities and multiple interaction sites, their inherent defects of poor mechanical strength and significant swelling tendency severely restrict their practical implementation in HPLC analysis. Thus, developing novel hydrogel-based stationary phases with excellent mechanical stability and efficient separation capability has become a key demand in this field. In this study, polyethyleneimine (PEI) hydrogel and silver nanoparticles (AgNPs) were successively anchored onto the silica microspheres to prepare a designed AgNPs/PEI nanocomposite hydrogel-functionalized silica stationary phase (AgNPs/PEI hydrogel@SiO2). By virtue of the strong coordination between the high-density amino groups in PEI and Ag+, stable anchoring of metal precursors and uniform dispersion of AgNPs were achieved, while the cross-linking degree of hydrogel was enhanced, simultaneously solving the problems of insufficient mechanical properties of hydrogel-based stationary phases. The AgNPs/PEI hydrogel@SiO2 stationary phase integrated multiple separation mechanisms and successfully achieved baseline separation of positional isomers, vitamins, nucleosides, and sulfonamides. Notably, the sulfonamides exhibited a typical mixed-mode chromatographic behavior, demonstrating superior retention strength and selectivity on the AgNPs/PEI hydrogel@SiO2 column compared to the commercial XAmide column. Ultimately, the AgNPs/PEI hydrogel@SiO2 was successfully applied to the detection of sulfonamides in lotion and lake water, confirming its reliability and accuracy for real sample analysis. This work introduces an innovative design concept for multifunctional HPLC stationary phases, overcoming the limitations of traditional hydrogel-based materials. With its excellent mechanical stability, versatile separation capabilities, and adaptability to complex samples, the AgNPs/PEI nanocomposite hydrogel offers an efficient solution for analyzing intricate systems, highlighting its significant scientific value and broad application potential in HPLC analysis.
{"title":"Polyethyleneimine hydrogel-silica composite with embedded silver nanoparticles as a multifunctional stationary phase for HPLC","authors":"Feng Hu, Qian Zhao, Qiaoling Liu, Yuefei Zhang, Wei Chen, Sheng Tang","doi":"10.1016/j.chroma.2026.466800","DOIUrl":"10.1016/j.chroma.2026.466800","url":null,"abstract":"<div><div>The development of chromatographic stationary phases remains a persistent focus of scientific inquiry, as their functions and properties directly determine separation efficiency and application scope. Although hydrogel-based stationary phases exhibit prominent advantages such as customizable functionalities and multiple interaction sites, their inherent defects of poor mechanical strength and significant swelling tendency severely restrict their practical implementation in HPLC analysis. Thus, developing novel hydrogel-based stationary phases with excellent mechanical stability and efficient separation capability has become a key demand in this field. In this study, polyethyleneimine (PEI) hydrogel and silver nanoparticles (AgNPs) were successively anchored onto the silica microspheres to prepare a designed AgNPs/PEI nanocomposite hydrogel-functionalized silica stationary phase (AgNPs/PEI hydrogel@SiO<sub>2</sub>). By virtue of the strong coordination between the high-density amino groups in PEI and Ag<sup>+</sup>, stable anchoring of metal precursors and uniform dispersion of AgNPs were achieved, while the cross-linking degree of hydrogel was enhanced, simultaneously solving the problems of insufficient mechanical properties of hydrogel-based stationary phases. The AgNPs/PEI hydrogel@SiO<sub>2</sub> stationary phase integrated multiple separation mechanisms and successfully achieved baseline separation of positional isomers, vitamins, nucleosides, and sulfonamides. Notably, the sulfonamides exhibited a typical mixed-mode chromatographic behavior, demonstrating superior retention strength and selectivity on the AgNPs/PEI hydrogel@SiO<sub>2</sub> column compared to the commercial XAmide column. Ultimately, the AgNPs/PEI hydrogel@SiO<sub>2</sub> was successfully applied to the detection of sulfonamides in lotion and lake water, confirming its reliability and accuracy for real sample analysis. This work introduces an innovative design concept for multifunctional HPLC stationary phases, overcoming the limitations of traditional hydrogel-based materials. With its excellent mechanical stability, versatile separation capabilities, and adaptability to complex samples, the AgNPs/PEI nanocomposite hydrogel offers an efficient solution for analyzing intricate systems, highlighting its significant scientific value and broad application potential in HPLC analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466800"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146256934","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2026-03-29Epub Date: 2026-02-03DOI: 10.1016/j.chroma.2026.466772
Imma Tolosa, David Huertas, Brigid Carr, Philippe Bersuder
This study developed and validated a multiresidue analytical procedure for sediment samples, targeting both legacy contaminants regulated under the UN Stockholm Convention on Persistent Organic Pollutants (POPs) and emerging contaminants of concern to marine ecosystems. The focus was on emerging plastic additives and flame retardants, such as phthalate esters (PAEs) and organophosphate esters (OPEs), for which limited data exists regarding their global presence or fate in the marine environment.
The methodology targets 6 marker PCBs, 20 organochlorinated pesticides (OCPs), 14 PBDEs, 17 alternative halogenated flame retardants (aHFRs), 19 PAEs, and 17 OPEs. The optimized procedure involves microwave extraction with a mixture of n-hexane and dichloromethane, sulfur clean-up with copper, and silica SPE fractionation to separate legacy POPs and aHFRs from PAEs and OPEs. Gas chromatography coupled with triple quadrupole mass spectrometry (GC-MS/MS) was used to measure the target analytes within two isolated fractions. Method validation included recovery yields in matrix-spiked sediments, reproducibility, repeatability, and blank optimization. Recoveries of PAEs and OPEs at 20-30 ng g−1 ranged within 62–120% for the majority of analytes with RSD< 25%. Method detection limits for PAEs and OPEs ranged from 0.03 ng/g to 12 ng/g dw, influenced by background contamination variability.
The validated method was applied to marine sediment samples, including reference materials from the International Atomic Energy Agency (IAEA), providing preliminary data on the occurrence of these compounds in the marine environment. Integrating the analysis of PAEs and OPEs into existing procedures for legacy contaminants offers a cost-effective approach to expanding data availability for emerging organic pollutants.
{"title":"A multiresidue analytical procedure for legacy and emerging organic contaminants in marine sediments: Method development, validation, and application","authors":"Imma Tolosa, David Huertas, Brigid Carr, Philippe Bersuder","doi":"10.1016/j.chroma.2026.466772","DOIUrl":"10.1016/j.chroma.2026.466772","url":null,"abstract":"<div><div>This study developed and validated a multiresidue analytical procedure for sediment samples, targeting both legacy contaminants regulated under the UN Stockholm Convention on Persistent Organic Pollutants (POPs) and emerging contaminants of concern to marine ecosystems. The focus was on emerging plastic additives and flame retardants, such as phthalate esters (PAEs) and organophosphate esters (OPEs), for which limited data exists regarding their global presence or fate in the marine environment.</div><div>The methodology targets 6 marker PCBs, 20 organochlorinated pesticides (OCPs), 14 PBDEs, 17 alternative halogenated flame retardants (aHFRs), 19 PAEs, and 17 OPEs. The optimized procedure involves microwave extraction with a mixture of n-hexane and dichloromethane, sulfur clean-up with copper, and silica SPE fractionation to separate legacy POPs and aHFRs from PAEs and OPEs. Gas chromatography coupled with triple quadrupole mass spectrometry (GC-MS/MS) was used to measure the target analytes within two isolated fractions. Method validation included recovery yields in matrix-spiked sediments, reproducibility, repeatability, and blank optimization. Recoveries of PAEs and OPEs at 20-30 ng g<sup>−1</sup> ranged within 62–120% for the majority of analytes with RSD< 25%. Method detection limits for PAEs and OPEs ranged from 0.03 ng/g to 12 ng/g dw, influenced by background contamination variability.</div><div>The validated method was applied to marine sediment samples, including reference materials from the International Atomic Energy Agency (IAEA), providing preliminary data on the occurrence of these compounds in the marine environment. Integrating the analysis of PAEs and OPEs into existing procedures for legacy contaminants offers a cost-effective approach to expanding data availability for emerging organic pollutants.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466772"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146155652","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2026-03-29Epub Date: 2026-02-14DOI: 10.1016/j.chroma.2026.466777
Jie Tian , Yi-fang Zhang , Yu-feng Sun , Dou Yan , Shuang Hu , Rong-rong Xing , Run-qin Wang , Li Yang , Xuan Chen
{"title":"Corrigendum to “A green and practical strategy for therapeutic drug monitoring of teicoplanin A2 components in human plasma using functionalized liquid film solvent bar microextraction coupled with high-performance liquid chromatography–ultraviolet detection” [Journal of Chromatography A 1768 (2026) 466673]","authors":"Jie Tian , Yi-fang Zhang , Yu-feng Sun , Dou Yan , Shuang Hu , Rong-rong Xing , Run-qin Wang , Li Yang , Xuan Chen","doi":"10.1016/j.chroma.2026.466777","DOIUrl":"10.1016/j.chroma.2026.466777","url":null,"abstract":"","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466777"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146199892","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2026-03-29Epub Date: 2026-02-15DOI: 10.1016/j.chroma.2026.466811
Dániel Tanács , Gábor Németi , Róbert Berkecz , Zsolt Bozsó , Gábor K. Tóth , Wolfgang Lindner , Antal Péter , István Ilisz
<div><div>In recent years, growing awareness of environmental sustainability has driven the search for eco-friendly alternatives in analytical chemistry. In liquid chromatography, this includes replacing traditional organic solvents like acetonitrile (MeCN) with greener options that comply with environmental standards while maintaining chromatographic performance. In this study, we describe in a comparative manner the performance of four <em>Cinchona</em> alkaloid-based ion-exchangers for the enantioresolution of fluorinated tryptophan analogs, applying dimethyl carbonate (DMC) as a green alternative to MeCN. Quinine- and quinidine-based zwitterionic chiral stationary phases (CSPs), namely ZWIX(+), ZWIX(–), ZWIX(+A), and ZWIX(–A) were utilized with binary mobile phase systems consisting of methanol (MeOH), MeCN, and DMC. To the best of our knowledge, this is the first report of the <em>Cinchona</em> alkaloid-based ion-exchangers applied with DMC-based mobile phase systems.</div><div>In polar ionic mode using MeOH/MeCN and MeOH/DMC mobile phases similar retention characteristics were obtained on all the <em>Cinchona</em>-based columns. Under the same eluent conditions, higher retention factors were observed in the presence of DMC, and in both systems, increasing the proportion of the less polar component (MeCN or DMC) in the mobile phase resulted in a significant increase in retention for all investigated tryptophan analogs, due to stronger interactions with the stationary phase. The stoichiometric displacement model described the dependence of retention on the counterion concentration with good accuracy in both mobile phase systems, and the more negative slopes observed in the case of DMC indicate the formation of stronger ionic interactions. Unlike in the MeCN-based system, the DMC-based eluents showed a general decrease in both enantioselectivity and resolution for most analytes as the DMC content increased on all four columns. Given the substantial difference in polarity between MeCN and DMC, notable variations in enantioselectivity were anticipated. Surprisingly, only modest deviations were detected when comparing mobile phases containing MeCN to those with DMC. Despite the similar chromatographic properties observed for the two solvents, the thermodynamic studies revealed significant differences between the two mobile phase systems. For MeCN-based eluents, retention times slightly decreased with temperature on most CSPs, in contrast, with DMC-based eluents, retention times increased for all analytes on all CSPs as temperature rose. Interesetingly, enantioselectivity changed differently on the studied CSPs; enthalpically driven separations were observed in the MeCN-containing systems on all zwitterionic CSPS, whereas several entropically driven separations were observed in the DMC-containing systems on the ZWIX(–) CSP. The elution order of the enantiomers remained unchanged, regardless of replacing MeCN with the greener solvent DMC or varying
{"title":"Comparative study of zwitterionic Cinchonane-based ion-exchangers for liquid chromatographic enantioseparations of free fluorinated tryptophanes: mechanistic and thermodynamic insights under green mobile phase conditions","authors":"Dániel Tanács , Gábor Németi , Róbert Berkecz , Zsolt Bozsó , Gábor K. Tóth , Wolfgang Lindner , Antal Péter , István Ilisz","doi":"10.1016/j.chroma.2026.466811","DOIUrl":"10.1016/j.chroma.2026.466811","url":null,"abstract":"<div><div>In recent years, growing awareness of environmental sustainability has driven the search for eco-friendly alternatives in analytical chemistry. In liquid chromatography, this includes replacing traditional organic solvents like acetonitrile (MeCN) with greener options that comply with environmental standards while maintaining chromatographic performance. In this study, we describe in a comparative manner the performance of four <em>Cinchona</em> alkaloid-based ion-exchangers for the enantioresolution of fluorinated tryptophan analogs, applying dimethyl carbonate (DMC) as a green alternative to MeCN. Quinine- and quinidine-based zwitterionic chiral stationary phases (CSPs), namely ZWIX(+), ZWIX(–), ZWIX(+A), and ZWIX(–A) were utilized with binary mobile phase systems consisting of methanol (MeOH), MeCN, and DMC. To the best of our knowledge, this is the first report of the <em>Cinchona</em> alkaloid-based ion-exchangers applied with DMC-based mobile phase systems.</div><div>In polar ionic mode using MeOH/MeCN and MeOH/DMC mobile phases similar retention characteristics were obtained on all the <em>Cinchona</em>-based columns. Under the same eluent conditions, higher retention factors were observed in the presence of DMC, and in both systems, increasing the proportion of the less polar component (MeCN or DMC) in the mobile phase resulted in a significant increase in retention for all investigated tryptophan analogs, due to stronger interactions with the stationary phase. The stoichiometric displacement model described the dependence of retention on the counterion concentration with good accuracy in both mobile phase systems, and the more negative slopes observed in the case of DMC indicate the formation of stronger ionic interactions. Unlike in the MeCN-based system, the DMC-based eluents showed a general decrease in both enantioselectivity and resolution for most analytes as the DMC content increased on all four columns. Given the substantial difference in polarity between MeCN and DMC, notable variations in enantioselectivity were anticipated. Surprisingly, only modest deviations were detected when comparing mobile phases containing MeCN to those with DMC. Despite the similar chromatographic properties observed for the two solvents, the thermodynamic studies revealed significant differences between the two mobile phase systems. For MeCN-based eluents, retention times slightly decreased with temperature on most CSPs, in contrast, with DMC-based eluents, retention times increased for all analytes on all CSPs as temperature rose. Interesetingly, enantioselectivity changed differently on the studied CSPs; enthalpically driven separations were observed in the MeCN-containing systems on all zwitterionic CSPS, whereas several entropically driven separations were observed in the DMC-containing systems on the ZWIX(–) CSP. The elution order of the enantiomers remained unchanged, regardless of replacing MeCN with the greener solvent DMC or varying","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466811"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146225058","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2026-03-29Epub Date: 2026-01-28DOI: 10.1016/j.chroma.2026.466752
Zhenhua Li , Qiaoling Zhao , Haoji Zhao , Tiejun Li , Hongmei Hu , Yuanming Guo , Heyong Cheng
As a class of the most prevalent broad-spectrum antibiotics, quinolones (QNs) are ubiquitous in various environmental matrices (in particular marine sediment). However, determination of multiple QNs in marine sediment is a challengeable task due to matrix complexity and strong QNs-sediment adsorption. Herein we presented an efficient quantification strategy for accurate measurement of 15 QNs in marine sediment based on ultrasonic extraction with 0.2 M Na2HPO4 in 50 v/v % acetonitrile, followed by automated solid-phase clean-up and ultra-performance liquid chromatography−tandem mass spectrometry with isotope dilution calibration. The method demonstrated negligible matrix effect, satisfactory recoveries (85 %–119 %), and low limits of detection (2–15 pg/g). Five QNs were detected in marine sediment from Yueqing Bay and Daiquyang with total concentrations of 5.6–12.1 μg/kg and 0.2–1.0 μg/kg, respectively, where four QNs including norfloxacin (NOR), enrofloxacin, ciprofloxacin, and ofloxacin were found in all samples, and NOR was the predominant compound both in Yueqing Bay and Daiquyang. Overall, the presented method is highly sensitive and reliable for routine quinolone analysis in marine sediment.
{"title":"Accurate quantification of quinolones in marine sediment by UPLC-MS/MS after ultrasonic extraction and automated SPE clean-up","authors":"Zhenhua Li , Qiaoling Zhao , Haoji Zhao , Tiejun Li , Hongmei Hu , Yuanming Guo , Heyong Cheng","doi":"10.1016/j.chroma.2026.466752","DOIUrl":"10.1016/j.chroma.2026.466752","url":null,"abstract":"<div><div>As a class of the most prevalent broad-spectrum antibiotics, quinolones (QNs) are ubiquitous in various environmental matrices (in particular marine sediment). However, determination of multiple QNs in marine sediment is a challengeable task due to matrix complexity and strong QNs-sediment adsorption. Herein we presented an efficient quantification strategy for accurate measurement of 15 QNs in marine sediment based on ultrasonic extraction with 0.2 M Na<sub>2</sub>HPO<sub>4</sub> in 50 v/v % acetonitrile, followed by automated solid-phase clean-up and ultra-performance liquid chromatography−tandem mass spectrometry with isotope dilution calibration. The method demonstrated negligible matrix effect, satisfactory recoveries (85 %–119 %), and low limits of detection (2–15 pg/g). Five QNs were detected in marine sediment from Yueqing Bay and Daiquyang with total concentrations of 5.6–12.1 μg/kg and 0.2–1.0 μg/kg, respectively, where four QNs including norfloxacin (NOR), enrofloxacin, ciprofloxacin, and ofloxacin were found in all samples, and NOR was the predominant compound both in Yueqing Bay and Daiquyang. Overall, the presented method is highly sensitive and reliable for routine quinolone analysis in marine sediment.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466752"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146099778","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2026-03-29Epub Date: 2026-02-11DOI: 10.1016/j.chroma.2026.466803
Nan Wang , Hao Qi , Shi-Lei Ji , Lu-Liang Wang
Selective detection of metformin (Glucophage) as an undeclared adulterant in health products is hampered by the complexity of sample matrices and the limitations of conventional adsorbents. While molecularly imprinted polymers (MIPs) offer specificity, they often suffer from low capacity and slow mass transfer. To overcome these challenges, a hierarchical adsorbent by grafting MIPs onto magnetic covalent organic frameworks (MCOFs) was engineered. MIPs@MCOFs substrate provided extensive surface area for high-density imprinting, while the magnetic core facilitates easy separation. MIPs@MCOFs exhibited high adsorption capacity (55.49 mg/g) and adsorption rate (40 min ) for Met. Based on this material, a reliable MSPE-HPLC method was established. It exhibited a wide linear range (5–10 , 000 μg/L), a low detection limit (1.1 μg/L), and satisfactory precision with intra- and inter-day RSDs below 2.2% and 6.5%, respectively. The method was validated for analyzing real samples, offering a powerful solution for combating illegal pharmaceutical adulteration in the health product industry.
{"title":"Molecularly imprinted magnetic covalent organic framework for selective extraction of metformin in health products","authors":"Nan Wang , Hao Qi , Shi-Lei Ji , Lu-Liang Wang","doi":"10.1016/j.chroma.2026.466803","DOIUrl":"10.1016/j.chroma.2026.466803","url":null,"abstract":"<div><div>Selective detection of metformin (Glucophage) as an undeclared adulterant in health products is hampered by the complexity of sample matrices and the limitations of conventional adsorbents. While molecularly imprinted polymers (MIPs) offer specificity, they often suffer from low capacity and slow mass transfer. To overcome these challenges, a hierarchical adsorbent by grafting MIPs onto magnetic covalent organic frameworks (MCOFs) was engineered. MIPs@MCOFs substrate provided extensive surface area for high-density imprinting, while the magnetic core facilitates easy separation. MIPs@MCOFs exhibited high adsorption capacity (55.49 mg/g) and adsorption rate (40 min ) for Met. Based on this material, a reliable MSPE-HPLC method was established. It exhibited a wide linear range (5–10 , 000 μg/L), a low detection limit (1.1 μg/L), and satisfactory precision with intra- and inter-day RSDs below 2.2% and 6.5%, respectively. The method was validated for analyzing real samples, offering a powerful solution for combating illegal pharmaceutical adulteration in the health product industry.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466803"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146218169","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2026-03-29Epub Date: 2026-01-29DOI: 10.1016/j.chroma.2026.466756
Wen-Jing Zhao, Xin-Yue Wang, Jin-Shuang Wang, Yuan-Yuan Cui, Cheng-Xiong Yang
In this work, a novel sulfonic acid-functionalized microporous organic network-coated SiO2 composite (SiO2@MON-SO3H-2) was synthesized for efficient solid-phase extraction (SPE) of quaternary ammonium alkaloids (QAAs) from complex traditional Chinese medicine (TCM) samples. The material exhibits a high specific surface area (381.4 m2 g−1), superhydrophilicity, and excellent stability. These properties, combined with synergistic interactions such as electrostatic attraction, hydrophobic effects, and π-π stacking, enabled the adsorbent to demonstrate outstanding extraction performance toward four typical QAAs. The developed method owns wide linear ranges (0.88–1000 μg L−1) with good linearity (R2 > 0.999), high sensitivity (limits of detection: 0.26–1.02 μg L−1), satisfactory precision (intra- and inter-day RSDs < 6.3%), high enhancement factors (> 91), and insignificant matrix effects (86.6–115.3%). The material maintained excellent reusability, with recoveries remaining above 89% after 50 extraction-desorption cycles. When applied to spiked herbal matrices, the method provided recoveries of 92.7–112.0%. SiO2@MON-SO3H-2 also gave higher recovery than commercial C18, activated carbon, macroporous adsorption resin AB-8, and the cation-exchange resin Amberlite 732. The present work demonstrates the prospect of SiO2@MON-SO3H-2 for trace QAAs extraction from complex samples and provides a reliable approach for TCM analysis and quality control.
{"title":"Efficient solid-phase extraction of quaternary ammonium alkaloids from traditional Chinese medicines on a novel sulfonic acid group functionalized microporous organic network coated SiO2 composite","authors":"Wen-Jing Zhao, Xin-Yue Wang, Jin-Shuang Wang, Yuan-Yuan Cui, Cheng-Xiong Yang","doi":"10.1016/j.chroma.2026.466756","DOIUrl":"10.1016/j.chroma.2026.466756","url":null,"abstract":"<div><div>In this work, a novel sulfonic acid-functionalized microporous organic network-coated SiO<sub>2</sub> composite (SiO<sub>2</sub>@MON-SO<sub>3</sub>H-2) was synthesized for efficient solid-phase extraction (SPE) of quaternary ammonium alkaloids (QAAs) from complex traditional Chinese medicine (TCM) samples. The material exhibits a high specific surface area (381.4 m<sup>2</sup> g<sup>−1</sup>), superhydrophilicity, and excellent stability. These properties, combined with synergistic interactions such as electrostatic attraction, hydrophobic effects, and π-π stacking, enabled the adsorbent to demonstrate outstanding extraction performance toward four typical QAAs. The developed method owns wide linear ranges (0.88–1000 μg L<sup>−1</sup>) with good linearity (R<sup>2</sup> > 0.999), high sensitivity (limits of detection: 0.26–1.02 μg L<sup>−1</sup>), satisfactory precision (intra- and inter-day RSDs < 6.3%), high enhancement factors (> 91), and insignificant matrix effects (86.6–115.3%). The material maintained excellent reusability, with recoveries remaining above 89% after 50 extraction-desorption cycles. When applied to spiked herbal matrices, the method provided recoveries of 92.7–112.0%. SiO<sub>2</sub>@MON-SO<sub>3</sub>H-2 also gave higher recovery than commercial C18, activated carbon, macroporous adsorption resin AB-8, and the cation-exchange resin Amberlite 732. The present work demonstrates the prospect of SiO<sub>2</sub>@MON-SO<sub>3</sub>H-2 for trace QAAs extraction from complex samples and provides a reliable approach for TCM analysis and quality control.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466756"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146099735","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2026-03-29Epub Date: 2026-02-11DOI: 10.1016/j.chroma.2026.466799
Giorgia Rinaldi , Danilo Donnarumma , Antonio Ferracane , Romana Rigger , Markus Obkircher , Mariosimone Zoccali , Luigi Mondello
Grapes are widely cultivated and consumed, requiring pesticide control to ensure consumer safety. Herein we report a simplified workflow for detecting 236 pesticides in white table grapes within the EU multi-annual control programme, along with chronic, acute and cumulative risk assessments. The method involved two complementary analytical platforms: low-pressure gas chromatography (LP-GC) for volatile/semi-volatile pesticides and ultra-high-performance liquid chromatography (UHPLC) for polar/thermally labile pesticides, both coupled to triple quadrupole mass spectrometry (QqQMS). The methods were validated in terms of linearity (correlation coefficients ≥0.998 for all analytes), extraction recovery (mean recoveries of 70–120 % for >90 % of pesticides), precision (intra- and inter-day relative standard deviations ≤20 % for all validated concentrations), trueness (in the range 63–135 %), and limit of quantification (ranging from 0.002 to 0.01 mg Kg-1 for LP-GC-QqQMS and from 0.002 to 0.05 mg Kg-1 for UHPLC-QqQMS). Analysis of 20 samples detected 23 pesticides, five of which exceeded MRLs. Risk assessment showed that parathion-methyl poses unacceptable chronic and acute risks (exceedance up to 234 % and 193 % respectively), especially for children under <10 years old and toddlers due to their high consumption and low body weight. This highlights the need for stricter monitoring and regulatory measures to minimize pesticide exposure to widely consumed fruits.
{"title":"Multiresidual analysis of pesticides in white table grapes using hyphenated chromatographic techniques: Compliance and risk assessment","authors":"Giorgia Rinaldi , Danilo Donnarumma , Antonio Ferracane , Romana Rigger , Markus Obkircher , Mariosimone Zoccali , Luigi Mondello","doi":"10.1016/j.chroma.2026.466799","DOIUrl":"10.1016/j.chroma.2026.466799","url":null,"abstract":"<div><div>Grapes are widely cultivated and consumed, requiring pesticide control to ensure consumer safety. Herein we report a simplified workflow for detecting 236 pesticides in white table grapes within the EU multi-annual control programme, along with chronic, acute and cumulative risk assessments. The method involved two complementary analytical platforms: low-pressure gas chromatography (LP-GC) for volatile/semi-volatile pesticides and ultra-high-performance liquid chromatography (UHPLC) for polar/thermally labile pesticides, both coupled to triple quadrupole mass spectrometry (QqQMS). The methods were validated in terms of linearity (correlation coefficients ≥0.998 for all analytes), extraction recovery (mean recoveries of 70–120 % for >90 % of pesticides), precision (intra- and inter-day relative standard deviations ≤20 % for all validated concentrations), trueness (in the range 63–135 %), and limit of quantification (ranging from 0.002 to 0.01 mg Kg<sup>-1</sup> for LP-GC-QqQMS and from 0.002 to 0.05 mg Kg<sup>-1</sup> for UHPLC-QqQMS). Analysis of 20 samples detected 23 pesticides, five of which exceeded MRLs. Risk assessment showed that parathion-methyl poses unacceptable chronic and acute risks (exceedance up to 234 % and 193 % respectively), especially for children under <10 years old and toddlers due to their high consumption and low body weight. This highlights the need for stricter monitoring and regulatory measures to minimize pesticide exposure to widely consumed fruits.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466799"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146218177","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2026-03-29Epub Date: 2026-02-10DOI: 10.1016/j.chroma.2026.466795
Sedigheh Makaremnia , Kamal Ghanemi
This study presents a silver-decorated boron-carbon-nitride (Ag@BCN) nanocomposite for ultra-rapid dispersive micro-solid-phase extraction (d-µ-SPE) of Hg(II) in diverse water samples, followed by detection using cold-vapor atomic absorption spectrometry (CVAAS). The material integrates the high surface area of a mesoporous BCN support with the high selectivity of Ag nanoparticles (60–75 nm) for Hg(II) through spontaneous amalgamation, addressing the kinetic and environmental limitations of traditional organic chelating agents. The developed D-µ-SPE method reached quantitative extraction equilibrium in just one minute, offering a substantial improvement over most existing D-µ-SPE techniques. The developed method demonstrated excellent analytical performance, with a low LOD (0.067 ng/mL), a high adsorption capacity (54.5 mg/g), and good precision (RSD < 4.6 %) under optimal conditions (pH 4.0, 70 mg of adsorbent). Additionally, the Ag@BCN adsorbent showed recoveries from 94.8 % to 100.0 % even in complex matrices of up to 5 % NaCl, demonstrating its stability in high-ionic-strength matrices like seawater and river water. By combining ultrafast kinetics monitoring, high sensitivity, and a user-friendly interface in a D-µ-SPE format, this work presents an efficient alternative to traditional methods for routine screening and monitoring of mercury in environmental waters.
{"title":"Silver-decorated boron carbon nitride nanocomposite for ultra-fast dispersive micro-solid-phase extraction and preconcentration of mercury (II) in environmental waters","authors":"Sedigheh Makaremnia , Kamal Ghanemi","doi":"10.1016/j.chroma.2026.466795","DOIUrl":"10.1016/j.chroma.2026.466795","url":null,"abstract":"<div><div>This study presents a silver-decorated boron-carbon-nitride (Ag@BCN) nanocomposite for ultra-rapid dispersive micro-solid-phase extraction (d-µ-SPE) of Hg(II) in diverse water samples, followed by detection using cold-vapor atomic absorption spectrometry (CVAAS). The material integrates the high surface area of a mesoporous BCN support with the high selectivity of Ag nanoparticles (60–75 nm) for Hg(II) through spontaneous amalgamation, addressing the kinetic and environmental limitations of traditional organic chelating agents. The developed D-µ-SPE method reached quantitative extraction equilibrium in just one minute, offering a substantial improvement over most existing D-µ-SPE techniques. The developed method demonstrated excellent analytical performance, with a low LOD (0.067 ng/mL), a high adsorption capacity (54.5 mg/g), and good precision (RSD < 4.6 %) under optimal conditions (pH 4.0, 70 mg of adsorbent). Additionally, the Ag@BCN adsorbent showed recoveries from 94.8 % to 100.0 % even in complex matrices of up to 5 % NaCl, demonstrating its stability in high-ionic-strength matrices like seawater and river water. By combining ultrafast kinetics monitoring, high sensitivity, and a user-friendly interface in a D-µ-SPE format, this work presents an efficient alternative to traditional methods for routine screening and monitoring of mercury in environmental waters.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1771 ","pages":"Article 466795"},"PeriodicalIF":4.0,"publicationDate":"2026-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146225140","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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