Pub Date : 2026-02-22Epub Date: 2025-12-17DOI: 10.1016/j.chroma.2025.466625
Mayada Elgohary , Alexandra L.J. Webb , Joseph C. Ward , Andal Murthy , Jack Hutchinson , James Button , George Thom , Philip Newton , Emmelie Hammarvid , Anna D. Baran , Juhi Patel , Hannah N. Turney , Mark J. Dickman , Sara Trabulo , Eivor Örnskov
Messenger RNA (mRNA) integrity is a critical quality attribute (CQA) commonly assessed using liquid chromatography (LC) and capillary gel electrophoresis (CGE). The LC and CGE methods used for integrity tests are also used for stability studies for establishing product shelf-life for mRNA-based therapeutics. Advances in sequence and structure engineering have demonstrated significant improvements in mRNA translatability and stability. However, the higher order structure (HOS) of mRNA remains poorly understood and it is difficult to correlate experimentally measured structures with their bioinformatically predicted conformations. Previous studies have shown that mRNA HOS can cause artefactual bands or peaks in CGE and LC analyses, leading to anomalous integrity readouts. In this study, we employed a range of biophysical methods to characterise mRNA HOS, aiming to clarify the origins of the additional peaks observed in CGE and LC analyses and to better comprehend the influences of predicted minimum free energy (MFE) and structural features on mRNA integrity, translatability, and stability. Our findings provide new method-related considerations for measuring mRNA integrity as well as insights into the effects of mRNA structure on stability under long term storage and forced degradation conditions.
{"title":"Biophysical characterisation of mRNA structure and its impact on integrity analysis by liquid chromatography and capillary gel electrophoresis methods","authors":"Mayada Elgohary , Alexandra L.J. Webb , Joseph C. Ward , Andal Murthy , Jack Hutchinson , James Button , George Thom , Philip Newton , Emmelie Hammarvid , Anna D. Baran , Juhi Patel , Hannah N. Turney , Mark J. Dickman , Sara Trabulo , Eivor Örnskov","doi":"10.1016/j.chroma.2025.466625","DOIUrl":"10.1016/j.chroma.2025.466625","url":null,"abstract":"<div><div>Messenger RNA (mRNA) integrity is a critical quality attribute (CQA) commonly assessed using liquid chromatography (LC) and capillary gel electrophoresis (CGE). The LC and CGE methods used for integrity tests are also used for stability studies for establishing product shelf-life for mRNA-based therapeutics. Advances in sequence and structure engineering have demonstrated significant improvements in mRNA translatability and stability. However, the higher order structure (HOS) of mRNA remains poorly understood and it is difficult to correlate experimentally measured structures with their bioinformatically predicted conformations. Previous studies have shown that mRNA HOS can cause artefactual bands or peaks in CGE and LC analyses, leading to anomalous integrity readouts. In this study, we employed a range of biophysical methods to characterise mRNA HOS, aiming to clarify the origins of the additional peaks observed in CGE and LC analyses and to better comprehend the influences of predicted minimum free energy (MFE) and structural features on mRNA integrity, translatability, and stability. Our findings provide new method-related considerations for measuring mRNA integrity as well as insights into the effects of mRNA structure on stability under long term storage and forced degradation conditions.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466625"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145973923","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}
A preconcentration and detection method using ionic liquid for embedded in melamine sponge for pipette tip micro solid-phase extraction of pyrethroid insecticides coupled to HPLC was developed for trace amount of pyrethroids residue detection. The synthesis of ionic liquid was accomplished by using tributylhexadecylphosphonium bromide ([P44412]Br) and potassium hexafluorophosphate (KPF6), after that effervescent process was carried out by adding sodium carbonate into a centrifuge tube. The as-prepared ionic liquid was then embedded into melamine sponge, and used for pipette tip micro solid-phase extraction of insecticides in fruit juice matrices. After impregnation, the morphological and structural properties of the sorbents were characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. Under the selected conditions, the method exhibited wide linear range (2 – 100 μg l-1) with a coefficient for determination (R2) greater than 0.99. The limit of quantification (LOQ) and limit of detection (LOD) were in the range of 2 – 3 μg l-1 and 0.7 – 1 μg l-1, respectively. Good reproducibility (RSD < 4.65%, n = 5) were achieved. Moreover, the proposed method provided high enrichment factors (EF) ranging from 36.50 to 45.52 folds. The sorbent was then applied to extract pyrethroids in fruit juice. Accuracy was excellent and acceptable recoveries were attained. The greenness profiles were evaluated utilizing multiple assessment metrics including the Analytical Eco-Scale, AGREE Assessment, and BAGI.
{"title":"Enrichment of pyrethroid insecticides using effervescent-assisted ionic liquid functionalized in melamine sponge for pipette tip micro solid-phase extraction","authors":"Dararat Saenkam , Pirom Suwannasom , Jitlada Vichapong","doi":"10.1016/j.chroma.2026.466674","DOIUrl":"10.1016/j.chroma.2026.466674","url":null,"abstract":"<div><div>A preconcentration and detection method using ionic liquid for embedded in melamine sponge for pipette tip micro solid-phase extraction of pyrethroid insecticides coupled to HPLC was developed for trace amount of pyrethroids residue detection. The synthesis of ionic liquid was accomplished by using tributylhexadecylphosphonium bromide ([P<sub>44412</sub>]Br) and potassium hexafluorophosphate (KPF<sub>6</sub>), after that effervescent process was carried out by adding sodium carbonate into a centrifuge tube. The as-prepared ionic liquid was then embedded into melamine sponge, and used for pipette tip micro solid-phase extraction of insecticides in fruit juice matrices. After impregnation, the morphological and structural properties of the sorbents were characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. Under the selected conditions, the method exhibited wide linear range (2 – 100 μg <span>l</span><sup>-1</sup>) with a coefficient for determination (R<sup>2</sup>) greater than 0.99. The limit of quantification (LOQ) and limit of detection (LOD) were in the range of 2 – 3 μg <span>l</span><sup>-1</sup> and 0.7 – 1 μg <span>l</span><sup>-1</sup>, respectively. Good reproducibility (RSD < 4.65%, <em>n</em> = 5) were achieved. Moreover, the proposed method provided high enrichment factors (EF) ranging from 36.50 to 45.52 folds. The sorbent was then applied to extract pyrethroids in fruit juice. Accuracy was excellent and acceptable recoveries were attained. The greenness profiles were evaluated utilizing multiple assessment metrics including the Analytical Eco-Scale, AGREE Assessment, and BAGI.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466674"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145909697","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 : 2026-02-22Epub Date: 2026-01-19DOI: 10.1016/j.chroma.2026.466719
Xujun Zhang , Shan Wang , Bo Sui , Yan Wang , Lingbo Ji , Jianxun Zhang , Ajuan Yu , Wu Fan , Wuduo Zhao
Desorption electrospray ionization mass spectrometry imaging (DESI-MSI) is regarded as a novel molecular imaging approach that integrates DESI source with conventional mass spectrometry to provide spatial information and molecular composition on the sample’s surface. In this review, the principle of DESI-MSI was elucidated, including its desorption process and ionization mechanism. Through the applications in biological tissues and organs, the advantages of DESI-MSI technology were demonstrated in exploring the tissue functional roles and disease mechanisms, including brain, liver, kidney, and lung. Building on these findings, we review DESI-MSI’s unique capability to map both exogenous and endogenous biomolecules, thereby providing insights into spatial distribution of exogenous organisms and endogenous metabolic of transformation pathways and pharmacokinetics. Finally, the recent applications of DESI-MSI in biomedicine, environmental monitoring, and food safety are also reviewed. With the continuous improvement of instruments and analysis methods, DESI-MSI is expected to bring meaningful changes across a growing number of fields, opening up exciting opportunities to support innovative technologies and applied research.
{"title":"Advances in desorption electrospray ionization mass spectrometry imaging: Research progress and applications","authors":"Xujun Zhang , Shan Wang , Bo Sui , Yan Wang , Lingbo Ji , Jianxun Zhang , Ajuan Yu , Wu Fan , Wuduo Zhao","doi":"10.1016/j.chroma.2026.466719","DOIUrl":"10.1016/j.chroma.2026.466719","url":null,"abstract":"<div><div>Desorption electrospray ionization mass spectrometry imaging (DESI-MSI) is regarded as a novel molecular imaging approach that integrates DESI source with conventional mass spectrometry to provide spatial information and molecular composition on the sample’s surface. In this review, the principle of DESI-MSI was elucidated, including its desorption process and ionization mechanism. Through the applications in biological tissues and organs, the advantages of DESI-MSI technology were demonstrated in exploring the tissue functional roles and disease mechanisms, including brain, liver, kidney, and lung. Building on these findings, we review DESI-MSI’s unique capability to map both exogenous and endogenous biomolecules, thereby providing insights into spatial distribution of exogenous organisms and endogenous metabolic of transformation pathways and pharmacokinetics. Finally, the recent applications of DESI-MSI in biomedicine, environmental monitoring, and food safety are also reviewed. With the continuous improvement of instruments and analysis methods, DESI-MSI is expected to bring meaningful changes across a growing number of fields, opening up exciting opportunities to support innovative technologies and applied research.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466719"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146023324","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 : 2026-02-22Epub Date: 2026-01-21DOI: 10.1016/j.chroma.2026.466725
Clara M.A. Eichler , Hannah Calder , Bharat Chandramouli , Matthew Curtis , Heidi Hayes , Benjamin Kim , Ruth Marfil-Vega , Cristina Matos Mejías , Laura Miles , Alan Owens , Jack Stuff , Kurt Thaxton , Jochen Vandenberg , Nicola Watson , David Wevill , Jackie A. Whitecavage , Xiaoyu Liu
Fluorotelomer alcohols (FTOHs) are a group of volatile and semi-volatile per- and polyfluoroalkyl substances (PFAS) commonly found in indoor air and contribute to PFAS inhalation exposure. Improving our understanding of the contribution of FTOHs to human exposure to PFAS indoors is of high interest. Consensus standard test methods play an essential role in environmental risk assessment and management. We present the outcome of an international interlaboratory study (ILS) conducted with nine laboratories to evaluate the precision of ASTM International Standard Test Method D8591. The ILS was organized by the United States Environmental Protection Agency. The test method specifies the analysis of four FTOHs (4:2, 6:2, 8:2 and 10:2 FTOH) collected on PFAS-specific thermal desorption tubes by gas chromatography coupled with tandem mass spectrometry. During the ILS, participating laboratories were instructed to use the test method to analyze three samples (A, B, and C), each three times. Each sample contained the target FTOHs at defined concentrations unknown to the laboratories. The results from seven laboratories show that the relative reproducibility standard deviation (RSDR) of the method ranges from 14% to 26% and the relative repeatability standard deviation (RSDr) ranges from 4.6% to 11%, with RSDs decreasing with decreasing volatility of the FTOHs. Bias ranged from -13% to 6.0% and was generally larger and negative for less volatile FTOHs. The test method in conjunction with the precision statistics from this ILS will provide a reliable, defendable method that can be used in the context of studying PFAS sources, transport, and human exposure.
{"title":"Measuring fluorotelomer alcohols by thermal desorption-gas chromatography-tandem mass spectrometry: Interlaboratory study results","authors":"Clara M.A. Eichler , Hannah Calder , Bharat Chandramouli , Matthew Curtis , Heidi Hayes , Benjamin Kim , Ruth Marfil-Vega , Cristina Matos Mejías , Laura Miles , Alan Owens , Jack Stuff , Kurt Thaxton , Jochen Vandenberg , Nicola Watson , David Wevill , Jackie A. Whitecavage , Xiaoyu Liu","doi":"10.1016/j.chroma.2026.466725","DOIUrl":"10.1016/j.chroma.2026.466725","url":null,"abstract":"<div><div>Fluorotelomer alcohols (FTOHs) are a group of volatile and semi-volatile per- and polyfluoroalkyl substances (PFAS) commonly found in indoor air and contribute to PFAS inhalation exposure. Improving our understanding of the contribution of FTOHs to human exposure to PFAS indoors is of high interest. Consensus standard test methods play an essential role in environmental risk assessment and management. We present the outcome of an international interlaboratory study (ILS) conducted with nine laboratories to evaluate the precision of ASTM International Standard Test Method D8591. The ILS was organized by the United States Environmental Protection Agency. The test method specifies the analysis of four FTOHs (4:2, 6:2, 8:2 and 10:2 FTOH) collected on PFAS-specific thermal desorption tubes by gas chromatography coupled with tandem mass spectrometry. During the ILS, participating laboratories were instructed to use the test method to analyze three samples (A, B, and C), each three times. Each sample contained the target FTOHs at defined concentrations unknown to the laboratories. The results from seven laboratories show that the relative reproducibility standard deviation (<em>RSD<sub>R</sub></em>) of the method ranges from 14% to 26% and the relative repeatability standard deviation (<em>RSD<sub>r</sub></em>) ranges from 4.6% to 11%, with RSDs decreasing with decreasing volatility of the FTOHs. Bias ranged from -13% to 6.0% and was generally larger and negative for less volatile FTOHs. The test method in conjunction with the precision statistics from this ILS will provide a reliable, defendable method that can be used in the context of studying PFAS sources, transport, and human exposure.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466725"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146023326","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 : 2026-02-22Epub Date: 2025-12-25DOI: 10.1016/j.chroma.2025.466654
Roberto Laganà Vinci , Carmelo Coppolino , Katia Arena , Francesco Cacciola , Patrik Appelblad , Paola Dugo , Luigi Mondello
Comprehensive two-dimensional liquid chromatography (LC × LC) offers unique opportunities to resolve structurally diverse analytes that cannot be fully characterized by conventional one-dimensional methods. In this work, different LC × LC configurations combining reversed-phase liquid chromatography (RP-LC) and hydrophilic interaction chromatography (HILIC) were systematically investigated for the separation of a 48-compound phenolic standard mixture. Special attention was devoted to the discussion of key method parameters affecting retention behaviour and selectivity in the different LC × LC configurations. Three setups, namely, HILIC × RP-LC, RP-LC × RP-LC, and RP-LC × HILIC were optimized using focusing modulation with active trapping and evaluated in terms of orthogonality, peak capacity, resolution, dilution factor, analysis time, and solvent consumption. Among the tested configurations, HILIC × RP-LC provided the best results in terms of both separation efficiency and operational sustainability with higher corrected peak capacity, reduced dilution, and enhanced throughput. On the one hand, RP-LC × RP-LC offered robust performance with broad applicability due to stationary-phase availability, whereas, RP-LC × HILIC showed complementary selectivity but lower eco-sustainability. The Red, Green, Blue (RGB) additive colour model was applied to integrate analytical, environmental, and productivity metrics, identifying HILIC × RP-LC as the most effective configuration. Finally, the optimized method was applied to the characterization of phenolic profiles in herbal liqueurs, enabling detailed fingerprinting of complex natural matrices. These findings highlight the importance of rationally selecting LC × LC configurations and demonstrate the potential of HILIC × RP-LC with focusing modulation for efficient, sustainable, and information-rich profiling of phenolic compounds.
{"title":"Scouting of different separation strategies for phenolic compounds in comprehensive two-dimensional liquid chromatography","authors":"Roberto Laganà Vinci , Carmelo Coppolino , Katia Arena , Francesco Cacciola , Patrik Appelblad , Paola Dugo , Luigi Mondello","doi":"10.1016/j.chroma.2025.466654","DOIUrl":"10.1016/j.chroma.2025.466654","url":null,"abstract":"<div><div>Comprehensive two-dimensional liquid chromatography (LC × LC) offers unique opportunities to resolve structurally diverse analytes that cannot be fully characterized by conventional one-dimensional methods. In this work, different LC × LC configurations combining reversed-phase liquid chromatography (RP-LC) and hydrophilic interaction chromatography (HILIC) were systematically investigated for the separation of a 48-compound phenolic standard mixture. Special attention was devoted to the discussion of key method parameters affecting retention behaviour and selectivity in the different LC × LC configurations. Three setups, namely, HILIC × RP-LC, RP-LC × RP-LC, and RP-LC × HILIC were optimized using focusing modulation with active trapping and evaluated in terms of orthogonality, peak capacity, resolution, dilution factor, analysis time, and solvent consumption. Among the tested configurations, HILIC × RP-LC provided the best results in terms of both separation efficiency and operational sustainability with higher corrected peak capacity, reduced dilution, and enhanced throughput. On the one hand, RP-LC × RP-LC offered robust performance with broad applicability due to stationary-phase availability, whereas, RP-LC × HILIC showed complementary selectivity but lower eco-sustainability. The Red, Green, Blue (RGB) additive colour model was applied to integrate analytical, environmental, and productivity metrics, identifying HILIC × RP-LC as the most effective configuration. Finally, the optimized method was applied to the characterization of phenolic profiles in herbal liqueurs, enabling detailed fingerprinting of complex natural matrices. These findings highlight the importance of rationally selecting LC × LC configurations and demonstrate the potential of HILIC × RP-LC with focusing modulation for efficient, sustainable, and information-rich profiling of phenolic compounds.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1769 ","pages":"Article 466654"},"PeriodicalIF":4.0,"publicationDate":"2026-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145883755","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 : 2026-02-08Epub Date: 2026-01-03DOI: 10.1016/j.chroma.2026.466673
Jie Tian , Yi-fang Zhang , Yu-feng Sun , Dou Yan , Shuang Hu , Rong-rong Xing , Run-qin Wang , Li Yang , Xuan Chen
A novel functionalized liquid film solvent bar microextraction (FLF-SBME) method coupled with high-performance liquid chromatography–ultraviolet detection (HPLC/UV) was developed for the extraction and subsequent determination of five A2-components of teicoplanin, TA2-1, TA2-2, TA2-3, TA2-4 and TA2-5, simultaneously in human plasma. The microextraction mechanism of FLF-SBME was systematically elucidated, in which tri-n-octyl methyl ammonium chloride (TOMAC) was employed to modify polypropylene hollow fibers (PP-HFs), enabling efficient enrichment and separation of the target analytes from plasma. The key extraction parameters influencing efficiency were thoroughly optimized. Under optimal conditions, the method provided high enrichment factors (36–59) for all five A2 components, along with good linearity (1.0–110 µg/mL; r > 0.99), limits of detection of 0.5–3.0 µg/mL, and lower limits of quantification of 1.0–5.0 µg/mL. The intra- and inter-day precision (RSD < 12.2 %) and accuracy (recoveries: 91.5–110.3 %) were satisfactory. With its notable enrichment capability, high selectivity, sensitivity, and reliability, the proposed FLF-SBME–HPLC/UV method is well-suited for the monitoring of teicoplanin in human plasma.
{"title":"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","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.2026.466673","DOIUrl":"10.1016/j.chroma.2026.466673","url":null,"abstract":"<div><div>A novel functionalized liquid film solvent bar microextraction (FLF-SBME) method coupled with high-performance liquid chromatography–ultraviolet detection (HPLC/UV) was developed for the extraction and subsequent determination of five A<sub>2</sub>-components of teicoplanin, TA<sub>2-1</sub>, TA<sub>2-2</sub>, TA<sub>2-3</sub>, TA<sub>2-4</sub> and TA<sub>2-5</sub>, simultaneously in human plasma. The microextraction mechanism of FLF-SBME was systematically elucidated, in which tri-<em>n</em>-octyl methyl ammonium chloride (TOMAC) was employed to modify polypropylene hollow fibers (PP-HFs), enabling efficient enrichment and separation of the target analytes from plasma. The key extraction parameters influencing efficiency were thoroughly optimized. Under optimal conditions, the method provided high enrichment factors (36–59) for all five A<sub>2</sub> components, along with good linearity (1.0–110 µg/mL; <em>r</em> > 0.99), limits of detection of 0.5–3.0 µg/mL, and lower limits of quantification of 1.0–5.0 µg/mL. The intra- and inter-day precision (RSD < 12.2 %) and accuracy (recoveries: 91.5–110.3 %) were satisfactory. With its notable enrichment capability, high selectivity, sensitivity, and reliability, the proposed FLF-SBME–HPLC/UV method is well-suited for the monitoring of teicoplanin in human plasma.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466673"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145931630","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 : 2026-02-08Epub Date: 2026-01-15DOI: 10.1016/j.chroma.2026.466709
Nazir Fattahi , Parvin Zohrabi , Pouya Karimi , Filipe Hobi Bordón Sosa , Beshare Hashemi , Fereshteh Shiri
Bisphenol A (BPA) is globally used in the plastic and polymer industries. Regarding its toxicity, it raises health and environmental concerns due to its potential leaching into water, soil, and food chains. This work aims to screen the most efficient terpene-based hydrophobic eutectic solvents (HESs) for the extraction of BPA using COSMO-RS, an in-silico predictive approach, thereby minimizing the need for extensive trial-and-error experimentation. We also evaluated the extraction efficiency of HESs by assessing the stability of hydrogen bonding using quantum chemistry calculations. A HES composed of menthol: octanoic acid (2:1) was found to be the most efficient solvent after experimental validations. Experimental design showed the optimal extraction conditions to be 95 µL of menthol: octanoic acid (2:1), 100 µL of KOH 4.5 M, and 100 µL of HCl 5.0 M. A maximum extraction recovery of 75% with a limit of detection of 0.05 µg/L was achieved under the optimal extraction conditions in a pH-switchable extraction process. The environmental impact and applicability of the method were subsequently evaluated using AGREE, AGREEprep, and the blue applicability grade index, scoring 0.61, 0.66, and 65.0, respectively.
{"title":"Screening terpene-based eutectic solvents for bisphenol A extraction from plastic-packed dairy products and water storage tanks: COSMO-RS and quantum chemistry calculations","authors":"Nazir Fattahi , Parvin Zohrabi , Pouya Karimi , Filipe Hobi Bordón Sosa , Beshare Hashemi , Fereshteh Shiri","doi":"10.1016/j.chroma.2026.466709","DOIUrl":"10.1016/j.chroma.2026.466709","url":null,"abstract":"<div><div>Bisphenol A (BPA) is globally used in the plastic and polymer industries. Regarding its toxicity, it raises health and environmental concerns due to its potential leaching into water, soil, and food chains. This work aims to screen the most efficient terpene-based hydrophobic eutectic solvents (HESs) for the extraction of BPA using COSMO-RS, an in-silico predictive approach, thereby minimizing the need for extensive trial-and-error experimentation. We also evaluated the extraction efficiency of HESs by assessing the stability of hydrogen bonding using quantum chemistry calculations. A HES composed of menthol: octanoic acid (2:1) was found to be the most efficient solvent after experimental validations. Experimental design showed the optimal extraction conditions to be 95 µL of menthol: octanoic acid (2:1), 100 µL of KOH 4.5 M, and 100 µL of HCl 5.0 M. A maximum extraction recovery of 75% with a limit of detection of 0.05 µg/L was achieved under the optimal extraction conditions in a pH-switchable extraction process. The environmental impact and applicability of the method were subsequently evaluated using AGREE, AGREEprep, and the blue applicability grade index, scoring 0.61, 0.66, and 65.0, respectively.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466709"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146034308","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}
Ganoderma lucidum triterpenoids (GLTs) are high-value bioactive metabolites with increasing demand in pharmaceutical and nutraceutical sectors. However, their structural diversity, characterized by numerous analogs and structural isomers, coupled with the complexity of sources such as spores, fruiting bodies, and mycelia, presents significant challenges for high-resolution separation and high-purity isolation. This review critically evaluates the evolution of chromatographic and preparative isolation technologies tailored for GLTs. We systematically analyze three integrated separation workflows, designated as Route I, II, and III, from a chromatographic perspective, focusing on how different stationary phase behaviors and mobile phase configurations address specific sample complexities. Key emerging technologies, including high-speed counter-current chromatography (HSCCC), and preparative supercritical fluid chromatography (Prep-SFC), are assessed for their efficacy in resolving isomeric pairs and reducing irreversible adsorption. Furthermore, a technical-economic and environmental evaluation using the environmental factor (E-factor) is provided to link separation efficiency with industrial purity requirements ranging from 30 % to 90 %. By comparing the resolution, throughput, and sustainability of these chromatographic modes, this review provides a strategic roadmap for selecting optimal purification platforms to ensure the quality standardization of Ganoderma lucidum products.
{"title":"Sustainable downstream processing of ganoderma lucidum triterpenoids: Integrated chromatographic strategies and techno-economic evaluation","authors":"Hui Wang , Nengqi Zhang , Houle Xiang , Jingwei Kou , Yuqing Zhang , Hanjie Ying , Pengpeng Yang , Hao Qiao , Jinglan Wu","doi":"10.1016/j.chroma.2026.466710","DOIUrl":"10.1016/j.chroma.2026.466710","url":null,"abstract":"<div><div><em>Ganoderma lucidum</em> triterpenoids (GLTs) are high-value bioactive metabolites with increasing demand in pharmaceutical and nutraceutical sectors. However, their structural diversity, characterized by numerous analogs and structural isomers, coupled with the complexity of sources such as spores, fruiting bodies, and mycelia, presents significant challenges for high-resolution separation and high-purity isolation. This review critically evaluates the evolution of chromatographic and preparative isolation technologies tailored for GLTs. We systematically analyze three integrated separation workflows, designated as Route I, II, and III, from a chromatographic perspective, focusing on how different stationary phase behaviors and mobile phase configurations address specific sample complexities. Key emerging technologies, including high-speed counter-current chromatography (HSCCC), and preparative supercritical fluid chromatography (Prep-SFC), are assessed for their efficacy in resolving isomeric pairs and reducing irreversible adsorption. Furthermore, a technical-economic and environmental evaluation using the environmental factor (E-factor) is provided to link separation efficiency with industrial purity requirements ranging from 30 % to 90 %. By comparing the resolution, throughput, and sustainability of these chromatographic modes, this review provides a strategic roadmap for selecting optimal purification platforms to ensure the quality standardization of <em>Ganoderma lucidum</em> products.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466710"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145973426","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 : 2026-02-08Epub Date: 2025-12-20DOI: 10.1016/j.chroma.2025.466641
Meiijian Wang , Hao Wang , Shiyun Lou , Dexi Tao , Yaolin Tang , Bingfang Zou , Yongqiang Wang
Liquid-phase microextraction (LPME) relies critically on precise solvent control to achieve efficient extractant recovery. To address this, we developed a magnetic microparticle-based dispersive liquid-phase microextraction (MP-DLPME) strategy, employing hydrophobic porous Fe3O4 microparticles (∼1 μm) as solvent-stabilizing microcarriers. These microparticles were functionalized via covalent grafting of 3-chloropropyltriethoxysilane (CPS) and optimized porosity, enabling rigid confinement of organic solvents (e.g., 1-octanol) through dual mechanisms: (I) hydrophobic solvent anchoring to modified surfaces and (II) capillary trapping within mesopores. When applied to hydrophobic polycyclic aromatic hydrocarbons (PAHs) and organophosphorus pesticides (OPPs), the system generates solvent-encapsulated magnetic aggregates that dynamically fragment into microdroplets under vortex-induced shear forces, facilitating efficient analyte extraction via magnetic collection. By integrating the high efficiency of dispersive extraction with the rapid recovery of magnetic separation, the MP-DLPME method provides a robust sample pretreatment solution for environmental water analysis.
{"title":"Engineered hydrophobic porous Fe3O4 microparticles for solvent-confined dispersive liquid-phase microextraction","authors":"Meiijian Wang , Hao Wang , Shiyun Lou , Dexi Tao , Yaolin Tang , Bingfang Zou , Yongqiang Wang","doi":"10.1016/j.chroma.2025.466641","DOIUrl":"10.1016/j.chroma.2025.466641","url":null,"abstract":"<div><div>Liquid-phase microextraction (LPME) relies critically on precise solvent control to achieve efficient extractant recovery. To address this, we developed a magnetic microparticle-based dispersive liquid-phase microextraction (MP-DLPME) strategy, employing hydrophobic porous Fe<sub>3</sub>O<sub>4</sub> microparticles (∼1 μm) as solvent-stabilizing microcarriers. These microparticles were functionalized via covalent grafting of 3-chloropropyltriethoxysilane (CPS) and optimized porosity, enabling rigid confinement of organic solvents (e.g., 1-octanol) through dual mechanisms: (I) hydrophobic solvent anchoring to modified surfaces and (II) capillary trapping within mesopores. When applied to hydrophobic polycyclic aromatic hydrocarbons (PAHs) and organophosphorus pesticides (OPPs), the system generates solvent-encapsulated magnetic aggregates that dynamically fragment into microdroplets under vortex-induced shear forces, facilitating efficient analyte extraction via magnetic collection. By integrating the high efficiency of dispersive extraction with the rapid recovery of magnetic separation, the MP-DLPME method provides a robust sample pretreatment solution for environmental water analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466641"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145831907","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 : 2026-02-08Epub Date: 2026-01-05DOI: 10.1016/j.chroma.2026.466671
Mengyuan Wang, Yunuo Fan, Ye Zhang, Ling Chen, Bin Li, Ping Li
The inherent chemodiversity and complexity of herbal products make their quality control extremely challenging. In this work, a comprehensive analysis strategy through combining a polarity-extended liquid chromatography-mass spectrometry system (4-in-1 analysis system) and a metabolite-oriented targeted screening algorithm (MetaboTarget) for herbal products was proposed. The 4-in-1 analytical technique significantly expanded detection coverage of analytes through polarity extension. The Python-based MetaboTarget algorithm constructs a predictive database of potential metabolites by integrating Phase I/II metabolic reaction rules with parent drug components absorbed into the blood. Using precursor ions for targeted DDA scanning of plasma samples enables comprehensive metabolite characterization through integration with feature-based molecular networking (FBMN). The developed strategy was successfully applied to the deep in vitro and in vivo analysis of chemical components of Gegen Qinlian Decoction (GQD). As a result, 303 components in GQD and 181 metabolites in plasma were annotated. This integrated strategy enables simultaneous detection of compounds across the full polarity spectrum (high/medium/low) while overcoming key challenges in metabolite identification through the MetaboTarget algorithm, which effectively addresses issues arising from strong endogenous interference and low target abundance, thereby providing a powerful tool for comprehensive characterization of complex herbal products.
{"title":"Enhanced metabolite profiling of herbal products using an integrated 4-in-1 analysis system and the MetaboTarget algorithm","authors":"Mengyuan Wang, Yunuo Fan, Ye Zhang, Ling Chen, Bin Li, Ping Li","doi":"10.1016/j.chroma.2026.466671","DOIUrl":"10.1016/j.chroma.2026.466671","url":null,"abstract":"<div><div>The inherent chemodiversity and complexity of herbal products make their quality control extremely challenging. In this work, a comprehensive analysis strategy through combining a polarity-extended liquid chromatography-mass spectrometry system (4-in-1 analysis system) and a metabolite-oriented targeted screening algorithm (MetaboTarget) for herbal products was proposed. The 4-in-1 analytical technique significantly expanded detection coverage of analytes through polarity extension. The Python-based MetaboTarget algorithm constructs a predictive database of potential metabolites by integrating Phase I/II metabolic reaction rules with parent drug components absorbed into the blood. Using precursor ions for targeted DDA scanning of plasma samples enables comprehensive metabolite characterization through integration with feature-based molecular networking (FBMN). The developed strategy was successfully applied to the deep <em>in vitro</em> and <em>in vivo</em> analysis of chemical components of Gegen Qinlian Decoction (GQD). As a result, 303 components in GQD and 181 metabolites in plasma were annotated. This integrated strategy enables simultaneous detection of compounds across the full polarity spectrum (high/medium/low) while overcoming key challenges in metabolite identification through the MetaboTarget algorithm, which effectively addresses issues arising from strong endogenous interference and low target abundance, thereby providing a powerful tool for comprehensive characterization of complex herbal products.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1768 ","pages":"Article 466671"},"PeriodicalIF":4.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145916404","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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