Journal of chromatography open最新文献

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Adsorption energy distributions: Theory and applications in liquid chromatography 吸附能量分布:液相色谱的理论与应用
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-09-02 DOI: 10.1016/j.jcoa.2025.100252
Abdul Haseeb , Yosief Wondmagegne , Miguel X. Fernandes , Jörgen Samuelsson
{"title":"Adsorption energy distributions: Theory and applications in liquid chromatography","authors":"Abdul Haseeb ,&nbsp;Yosief Wondmagegne ,&nbsp;Miguel X. Fernandes ,&nbsp;Jörgen Samuelsson","doi":"10.1016/j.jcoa.2025.100252","DOIUrl":"10.1016/j.jcoa.2025.100252","url":null,"abstract":"<div><div>In liquid chromatography (LC), adsorption heterogeneity arises from the distribution of adsorption sites on stationary phases with varying interaction energies, affecting retention and separation performance. This heterogeneity can cause peak tailing, reduced resolution, and unpredictable retention times in analytical chromatography, as well as broad, asymmetric elution profiles in preparative systems. Adsorption heterogeneity depends on the combined effects of the stationary phase, the mobile phase composition, the analyte properties, and the chromatographic conditions. Traditional adsorption isotherms often fail to fully describe these complex interactions because they assume uniform adsorption energies.</div><div>The Adsorption Energy Distribution (AED) framework offers a powerful alternative by modelling adsorption as a sum of independent homogeneous sites, each with a specific energy, offering a realistic representation of heterogeneous adsorption. This review introduces the theoretical foundations of AED, including its mathematical formulation and computational approaches, and discusses its application in interpreting retention mechanisms in LC. AED analysis is illustrated through its use in both chiral and achiral separations, as well as its ability to explain peak tailing and surface heterogeneity. Practical considerations, such as the range of concentration data in the adsorption isotherm, the selection of a suitable kernel function, and the number of iterations and grid points in AED analysis, are discussed. Special emphasis is given on how to visualize and interpret the AED. This review aims to provide chromatographers with a comprehensive understanding of AED, emphasizing its practical value in characterizing the chromatographic system and elucidating retention mechanisms in liquid chromatography.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100252"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145004271","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Interaction properties and separation potential of zwitterionic stationary phases in hydrophilic interaction liquid chromatography 亲水相互作用液相色谱中两性离子固定相的相互作用性质和分离电位
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-09-15 DOI: 10.1016/j.jcoa.2025.100258
Zuzana Vosáhlová , Jana Poláchová , Jiří Svoboda , Michal Kohout , Květa Kalíková
{"title":"Interaction properties and separation potential of zwitterionic stationary phases in hydrophilic interaction liquid chromatography","authors":"Zuzana Vosáhlová ,&nbsp;Jana Poláchová ,&nbsp;Jiří Svoboda ,&nbsp;Michal Kohout ,&nbsp;Květa Kalíková","doi":"10.1016/j.jcoa.2025.100258","DOIUrl":"10.1016/j.jcoa.2025.100258","url":null,"abstract":"<div><div>Two commercially available zwitterionic columns, one diol-based column and two newly developed experimental zwitterionic columns for hydrophilic interaction liquid chromatography (HILIC) were characterized and compared in terms of their interaction abilities. The novel HILIC columns offer mixed-mode cation-exchange and anion-exchange interactions together with minor hydrophobic contribution of alkyl spacers between the units.</div><div>Tanaka testing protocol, which provides complex information about column retentivity, hydrophobicity, hydrophilicity and cation/anion-exchange characters was performed. The results revealed the differences between individual zwitterionic stationary phases and clear predominance of cation-exchange character over anion-exchange character was observed for all tested columns. The measurements at different pH at various buffer salt concentrations revealed that the predominance of negative charge on the stationary phase surface occurs at pH 4.7 and higher (probably due to the dissociation of residual silanols). At lower pH (pH 3.0) the anion-exchange mechanism also applies. The cation-exchange character (applying across the whole pH range) has been further studied using other simple chromatographic tests and compared with &gt;20 other commercially available columns. The application potential of all the tested columns was verified for analysis of tryptophan and its derivatives and also for cytochrome C tryptic digests.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100258"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145104205","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Method for the simultaneous enantioselective analysis of 21 natural amino acids and its application to analytics of fluorenylmethoxycarbonyl-derivatives under liquid chromatography conditions 21种天然氨基酸同时对映选择分析方法及其在液相色谱条件下分析氟酰甲氧羰基衍生物中的应用
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-11-11 DOI: 10.1016/j.jcoa.2025.100286
Antoine Falatas, Nicolas Hausser, Léa Kinderstuth, Mireille Schaeffer, Pilar Franco
{"title":"Method for the simultaneous enantioselective analysis of 21 natural amino acids and its application to analytics of fluorenylmethoxycarbonyl-derivatives under liquid chromatography conditions","authors":"Antoine Falatas,&nbsp;Nicolas Hausser,&nbsp;Léa Kinderstuth,&nbsp;Mireille Schaeffer,&nbsp;Pilar Franco","doi":"10.1016/j.jcoa.2025.100286","DOIUrl":"10.1016/j.jcoa.2025.100286","url":null,"abstract":"<div><div>The aim of this short communication is to show effective solutions for the control of enantiomeric excess simultaneously on free and protected amino acids (AAs). Such development has interest in the easy implementation of QC control of raw materials in peptide synthesis. Enantiomeric purity of Fmoc-<span>l</span>-AAs (containing fluorenylmethoxycarbonyl amine protecting group) is controlled on a routine base to determine the content of the Fmoc <span>d</span>-counterpart which can be present as impurity. However, the current analytical methods do not allow the simultaneous determination of potential unprotected <span>l</span>- and <span>d</span>-AAs which can be also present as impurities (in the same sample). The analytical conditions described in this publication were specifically achieved on a single ionic chiral column offering enantiomeric selectivity for free AAs derivatized with AQC (6-aminoquinolyl-N-hydroxysuccinimidyl carbamate) and for Fmoc-protected AAs. Only Fmoc-Proline quality control required the use of a different column, but with a similar mobile phase. The proposed methods enable both total and enantioselective AA quantification in a single chromatographic run. The workflow includes pre-column derivatization of the free AAs and optimization of chromatographic conditions for both derivatized and protected AA versions to be resolved in their enantiomeric forms in the same run. Representative results for the resolution of 21 AAs as AQC-derivatives are shown along with their retention behaviour. Subsequently, the analysis of every Fmoc-AA with their protected and unprotected chiral impurities is presented. The methods provide high resolution and selectivity as well as good reproducibility, which will facilitate efficient AAs profiling in diverse matrices.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100286"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145578664","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Integrating ultrashort-chain compounds into the comprehensive analysis of per- and polyfluorinated substances in ready-to-feed liquid milk samples 将超短链化合物整合到对即食液态奶样品中全氟和多氟物质的综合分析中
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-08-14 DOI: 10.1016/j.jcoa.2025.100246
Shun-Hsin Liang, Justin A. Steimling
{"title":"Integrating ultrashort-chain compounds into the comprehensive analysis of per- and polyfluorinated substances in ready-to-feed liquid milk samples","authors":"Shun-Hsin Liang,&nbsp;Justin A. Steimling","doi":"10.1016/j.jcoa.2025.100246","DOIUrl":"10.1016/j.jcoa.2025.100246","url":null,"abstract":"<div><div>Ultrashort-chain (USC) per- and polyfluoroalkyl substances (PFAS) are highly polar compounds with carbon chains shorter than C4. Their widespread occurrence in aquatic environments has raised growing concerns about potential contamination in food products, particularly ready-to-feed liquid milk. To fully assess and mitigate PFAS contamination, it is essential to include USC compounds in PFAS analysis of milk samples. The high polarity of USC PFAS poses a significant challenge for standard chromatographic practices in PFAS analysis, primarily due to insufficient chromatographic retention. This study introduces a simple and reliable workflow for the simultaneous analysis of C1 to C14 perfluoroalkyl carboxylic and sulfonic acids, along with other PFAS classes, in various liquid milk matrices. The chromatographic analysis was performed using an inert-coated polar-embedded alkyl phase LC column. Method verification was conducted using three different milk types—dairy milk, almond milk, and infant formula—to demonstrate the workflow’s applicability for measuring 41 PFAS in diverse milk samples. A sample preparation procedure involving protein precipitation, extractant drying, and reconstitution was optimized for the effective extraction and quantification of all analytes. This streamlined procedure was evaluated by accuracy and precision analysis at five fortification levels, ranging from 0.01 to 0.25 µg/kg, equivalent to 10 to 250 ng/L in the final sample solution for LC-MS/MS analysis. Eighteen isotopes, serving as quantitative internal standards, were added to the sample before extraction to ensure accurate quantification by correcting variations in sample preparation, matrix effects, and instrument response. Calibration ranges varied among different analytes, spanning from 4 – 2500 ng/L. All analytes exhibited recovery values within 30 % of the nominal concentration across all fortification levels. Satisfactory method precision was demonstrated with %RSD values below 15 %. The established workflow was then applied to the analysis of additional milk samples collected from various grocery stores, providing a comprehensive profile of PFAS contamination across a diverse range of milk matrices.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100246"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144866480","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Rapid High Performance Liquid Chromatography methodologies for analytical characterization of biotherapeutic products 生物治疗产品分析表征的快速高效液相色谱方法
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-10-16 DOI: 10.1016/j.jcoa.2025.100272
Anurag S. Rathore, Debasmita Chakraborty, Deepika Sarin
{"title":"Rapid High Performance Liquid Chromatography methodologies for analytical characterization of biotherapeutic products","authors":"Anurag S. Rathore,&nbsp;Debasmita Chakraborty,&nbsp;Deepika Sarin","doi":"10.1016/j.jcoa.2025.100272","DOIUrl":"10.1016/j.jcoa.2025.100272","url":null,"abstract":"<div><div>The last two decades have witnessed an increasing interest in rapid analytical methods amongst the biopharmaceutical industry. This interest has, in turn, resulted in advancements in analytical hardware, data analytics, and practices. In this article, we review major developments that have occurred over the last 6 years (2019–2025) in rapid chromatographic analysis of proteins, including monoclonal antibodies (mAbs), antibody-drug conjugates (ADCs), and other therapeutic proteins. Conventional high-performance liquid chromatography (HPLC) is vital for characterizing critical quality attributes (CQAs), but has limitations like long run times, manual handling, and low throughput. Recent developments in rapid HPLC have given a new direction to biopharmaceutical analysis by reducing analysis times from hours to minutes, while maintaining resolution and sensitivity. Key aspects of improvements that have been addressed in this review include chromatography equipment, column innovations, and advanced methodologies that have contributed towards the implementation of rapid HPLC methods in the biopharmaceutical industry. Furthermore, integrating process analytical technology (PAT) with rapid HPLC has made it possible to monitor CQAs in real-time, either inline or at-line, which is crucial for manufacturers engaged in continuous processing. The review also discusses data analytics and software-driven method development, which have significantly lowered experimental efforts and strengthened method reliability. The article focuses mainly on rapid HPLC-based analysis and does not include the mass spectrometry (MS) oriented faster analytical methods.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100272"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145361929","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Nanotechnology in bioanalysis: Current trends and applications 纳米技术在生物分析中的应用
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-09-03 DOI: 10.1016/j.jcoa.2025.100254
Arshdeep Chopra , Yogindra Kumari , Samarth Kumar , Renuka Sharma , Rohit Bhatia
{"title":"Nanotechnology in bioanalysis: Current trends and applications","authors":"Arshdeep Chopra ,&nbsp;Yogindra Kumari ,&nbsp;Samarth Kumar ,&nbsp;Renuka Sharma ,&nbsp;Rohit Bhatia","doi":"10.1016/j.jcoa.2025.100254","DOIUrl":"10.1016/j.jcoa.2025.100254","url":null,"abstract":"<div><div>Nanotechnology has evolved into an interdisciplinary trend spanning nearly all scientific domains and has had a profound impact on the global community over the last decade. On the surface, miniaturisation offers mechanical, chemical, and biological components that operate more quickly and affordably. Through the development of new nanoparticles (NPs), nanodevices, nanosensors, and nanosorbents for analytical procedures, the inclusion of nanotechnology has additionally had an impact on bioanalytical sciences. In recent years, numerous studies have been done on the integration of nanomaterials and their analysis in various biological samples. Given the scope of the NPs integrated bioanalysis, the purpose of this review is to provide an overview of multiple types of extraction techniques, sample preparation, and nanomaterials like magnetic NPs, carbon-based NPs, molecularly implanted polymers (MIPs) used in the determination of different drugs in biological specimens, and also to critically evaluate the tools used to examine Green Analytical Chemistry (GAC), such as Green Analytical Procedure Index (GAPI), ComplexGAPI (CoGAPI), Click Analytical Chemistry Index (CACI).</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100254"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145049342","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Predicting enantioseparations on polysaccharide-based stationary phases using achiral and chiral molecular descriptors 利用非手性和手性分子描述符预测多糖基固定相的对映体分离
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-10-28 DOI: 10.1016/j.jcoa.2025.100279
Pieter De Gauquier , Jordy Peeters , Fardine Ameli , Emmanuelle Lipka , Kenno Vanommeslaeghe , Yvan Vander Heyden , Debby Mangelings
{"title":"Predicting enantioseparations on polysaccharide-based stationary phases using achiral and chiral molecular descriptors","authors":"Pieter De Gauquier ,&nbsp;Jordy Peeters ,&nbsp;Fardine Ameli ,&nbsp;Emmanuelle Lipka ,&nbsp;Kenno Vanommeslaeghe ,&nbsp;Yvan Vander Heyden ,&nbsp;Debby Mangelings","doi":"10.1016/j.jcoa.2025.100279","DOIUrl":"10.1016/j.jcoa.2025.100279","url":null,"abstract":"<div><div>Achiral and chiral molecular descriptors were used to build models that predict the global retention of chiral molecules on the one hand, and their enantioselectivity, separation and elution sequence on the other. Chromatographic separations of 48 structurally diverse molecules were performed on six polysaccharide-based chiral stationary phases (CSPs) with two mobile phases (i.e. twelve chromatographic systems). Subsequently, “achiral” and “chiral” models were constructed. For the achiral models, either the mean retention time of the enantiomers (<span><math><mover><mrow><msub><mi>t</mi><mi>R</mi></msub></mrow><mo>‾</mo></mover></math></span>) or the logarithm of the mean retention factor (log <span><math><mover><mi>k</mi><mo>¯</mo></mover></math></span>) was modelled as a function of achiral descriptors, whereas for chiral models, the enantioselectivity was modelled using “Ensemble Steric and Electrostatic Chirality” (ESEC) descriptors. Initially, various types of ESEC descriptors were used to create models. A variable reduction technique, known as the Variable - Wootton, Sergent, Phan-Tan-Luu’s (V-WSP) algorithm, was applied to discard highly correlated descriptors. Stepwise multiple linear regression was applied to build the models. The achiral models for log <span><math><mover><mi>k</mi><mo>¯</mo></mover></math></span> predicted the global retention rather well. For the enantioselectivity, separation and elution sequence, chiral models with good performance parameters and predictive abilities were obtained. Finally, the results from the achiral and chiral models were combined to predict the retention times of individual enantiomers. Predicted chromatograms were generated, to visualize both the expected and experimental separation. In most cases, the combined models yielded a moderate error (median relative error ranged from 5.8% to 22% across all systems) for the individual enantiomers.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100279"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145473832","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Application of alrestatin chloride as a derivatizing reagent for the determination of amino acids, catecholamines and biogenic amines in urine 氯阿司他汀衍生试剂在测定尿液中氨基酸、儿茶酚胺和生物胺中的应用
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-10-07 DOI: 10.1016/j.jcoa.2025.100268
A. Temerdashev , A. Azaryan , Dzh. Konshina , V. Konshin , M. Steshin , E. Gashimova , S.N. Atapattu , Y.-Q. Feng , Q.-F. Zhu
{"title":"Application of alrestatin chloride as a derivatizing reagent for the determination of amino acids, catecholamines and biogenic amines in urine","authors":"A. Temerdashev ,&nbsp;A. Azaryan ,&nbsp;Dzh. Konshina ,&nbsp;V. Konshin ,&nbsp;M. Steshin ,&nbsp;E. Gashimova ,&nbsp;S.N. Atapattu ,&nbsp;Y.-Q. Feng ,&nbsp;Q.-F. Zhu","doi":"10.1016/j.jcoa.2025.100268","DOIUrl":"10.1016/j.jcoa.2025.100268","url":null,"abstract":"<div><div>The feasibility of using alrestatin chloride as a derivatization reagent was evaluated. Selected amino acids, catecholamines, and biogenic amines were tested. Limits of detection (LOD), limits of quantification (LOQ), and key analytical performance parameters were determined. Depending on the analyte, the detection limit varied from 0.1 to 5 ng/ml, and the error did not exceed 15 %, which allows the effective use of alrestatin chloride as a derivatizing reagent and significantly exceeds FMOC<img>Cl and dansyl chloride in sensitivity. An important advantage established for these derivatives is that they are stable over a long period of time. A proposed interpretation of the amino acid derivative is presented, and optimal MRM transitions for quantitative and qualitative analysis are established. It is shown that, although the proposed derivatization approach provides high sensitivity, prolonged heating is required to ensure a complete derivatization reaction, which can negatively impact analyte stability.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100268"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145324678","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Orthogonality of separation and sorbent evaluation in offline multidimensional peptide fractionation using automated positive pressure micro solid phase extraction 自动正压微固相萃取脱机多维肽分馏中分离的正交性及吸附剂评价
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-09-24 DOI: 10.1016/j.jcoa.2025.100262
Renata Biba , Karla Košpić , Blaž Ivšić , Lucija Vujević , Amela Hozić , Marijana Erk , Irena Đapić , Mario Cindrić
{"title":"Orthogonality of separation and sorbent evaluation in offline multidimensional peptide fractionation using automated positive pressure micro solid phase extraction","authors":"Renata Biba ,&nbsp;Karla Košpić ,&nbsp;Blaž Ivšić ,&nbsp;Lucija Vujević ,&nbsp;Amela Hozić ,&nbsp;Marijana Erk ,&nbsp;Irena Đapić ,&nbsp;Mario Cindrić","doi":"10.1016/j.jcoa.2025.100262","DOIUrl":"10.1016/j.jcoa.2025.100262","url":null,"abstract":"<div><div>Micro solid-phase extraction (µSPE) is a simple and efficient method for peptide separation, purification, and fractionation prior to mass spectrometry (MS) in bottom-up proteomics workflows. Here, we introduce a positive-pressure (PP)-µSPE platform for offline multidimensional peptide fractionation. Six one-dimensional (1D) fractionation protocols were optimized at low pH reversed-phase (RP), high pH RP, strong cation exchange (SCX), hydrophilic-lipophilic balance (HLB), quaternary methyl-ammonium (QMA), and mixed strong anion exchange/reversed-phase (MAX) using bovine serum albumin (BSA) tryptic peptides. Each protocol yielded six fractions, which were evaluated by peptide size, isoelectric point, and hydrophilicity. Peptide fractions were separated on nano-C18 RP column and analyzed by nanoESI-QTOF-MS, and fractionation performance was subsequently evaluated for each fractionation mode. The data were then paired to quantify orthogonality in projected multidimensional fractionation by employing information theory. QMA yielded the highest entropy, indicating the greatest peptide dispersion in 1D. Conversely, high pH RP fractionation had the lowest entropy and led to increased peptide modification and aggregation, compromising downstream analysis. Joint entropy and mutual information analysis identified the most orthogonal pairings (QMA–low pH RP, MAX–QMA, HLB–QMA) and highlighted redundancy among methods sharing similar separation mechanisms. Workflow’s practical utility was demonstrated on the fragment antigen-binding part of Cetuximab, where QMA fractionation enabled identification of a previously undetected heavy chain peptide, achieving complete sequence coverage. These results demonstrate that PP-µSPE enables repeatable and combinable peptide fractionation across diverse sorbents and complex proteins, and supports targeted workflows by facilitating selective peptide isolation based on their physicochemical properties, streamlining experimental design in multidimensional proteomic analyses.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100262"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145218999","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Comprehensive two-dimensional gas chromatography analysis of volatiles on e-liquids and aerosol compounds produced during the heating process 综合二维气相色谱分析在加热过程中产生的电子液体和气溶胶化合物的挥发物
IF 3.2
Journal of chromatography open Pub Date : 2025-11-01 Epub Date: 2025-10-18 DOI: 10.1016/j.jcoa.2025.100273
Glaucimar Alex Passos Resende , Sofia Madruga Marcondes Ferraz , Lucas Paines Bressan , Isadora de Oliveira , Thiago Nazario , Lucas Pessôa de Araujo , Leandro Wang Hantao
{"title":"Comprehensive two-dimensional gas chromatography analysis of volatiles on e-liquids and aerosol compounds produced during the heating process","authors":"Glaucimar Alex Passos Resende ,&nbsp;Sofia Madruga Marcondes Ferraz ,&nbsp;Lucas Paines Bressan ,&nbsp;Isadora de Oliveira ,&nbsp;Thiago Nazario ,&nbsp;Lucas Pessôa de Araujo ,&nbsp;Leandro Wang Hantao","doi":"10.1016/j.jcoa.2025.100273","DOIUrl":"10.1016/j.jcoa.2025.100273","url":null,"abstract":"<div><div>Electronic cigarettes (e-cigarettes) have gained global popularity, raising public health concerns due to the limited regulation and chemical complexity of e-liquids and their aerosols. This study presents the compositional analysis of volatile and semi-volatile organic compounds in 34 commercial e-liquid samples and their corresponding aerosols using headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography coupled with mass spectrometry (GC×GC–MS). The HS-SPME method was optimized using a central composite design (CCD), which established the ideal extraction conditions. One hundred twenty-six compounds were identified in the e-liquids. Chemometric analysis revealed distinct flavor profiles. The occurrence of concerning aldehydes, including benzaldehyde and (E)-cinnamaldehyde, was confirmed in the samples. The study of compounds generated when the e-liquids were heated at various temperatures (190–270 °C) and durations (3–30 min) showed the formation of harmful and potentially harmful constituents (HPHCs), including furfural, glycidol, and diacetyl, under specific conditions. Principal component analysis (PCA) of the aerosol data revealed the impact of heating time on the volatilization of both major e-liquid components and lower-concentration flavoring compounds. Overall, this study demonstrated the potential of GC×GC–MS for characterizing e-liquids and enhanced our understanding of toxic compound formation during the heating of e-liquids.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100273"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145361932","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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