Mirna Maalouf , Mateusz Janek , Enrico Friedrich , Nicolas Hausser , Jesse Bischof , Michael Lämmerhofer
{"title":"Bioinert chiral columns with Dursan-coated stainless-steel hardware for enantioselective liquid chromatography of polar analytes","authors":"Mirna Maalouf , Mateusz Janek , Enrico Friedrich , Nicolas Hausser , Jesse Bischof , Michael Lämmerhofer","doi":"10.1016/j.jcoa.2026.100347","DOIUrl":"10.1016/j.jcoa.2026.100347","url":null,"abstract":"<div><div>Analyte interactions with metal surfaces of column hardware are a well-known source of peak tailing, carry-over and poor recovery, particularly for polar compounds with chelating properties that have a high metal affinity and surface adsorption potential like phosphonic acids, amino acids and hydroxy carboxylic acids. While biocompatible and bioinert column hardware has emerged as a promising solution for non-chiral liquid chromatography, its impact on enantioselective chromatography remains underexplored. In this study, two quinine carbamate based chiral stationary phases, CHIRALPAK QN-AX and ZWIX(+), were evaluated in both Dursan-coated and conventional uncoated stainless steel column hardware. Dursan is a functionalized amorphous silicon oxide coating leading to chemical inertness and was tested herein for its ability to improve the enantioseparation performance of amino acids, amino phosphonic and phosphinic acids and hydroxy carboxylic acids. For the majority of amino acid enantioseparations reduced peak width, improved resolution and less tailing could be realized on ZWIX(+). The most pronounced benefits were observed for an aminophosphonic acid while the positive effect was moderate for a corresponding aminophosphinic acid. An improvement in chromatographic performance with Dursan-coated hardware was also found for the more hydrophilic hydroxy carboxylic acid enantiomer separations (2-hydroxyglutarate, lactate) on QN-AX while the effect was negligible for less hydrophilic congeners. These findings highlight the compound-specific nature of surface interactions and underscore the value of chemically inert column hardware in enantioselective LC. Overall, the study supports the use of Dursan-coated columns as a viable strategy for advancing bioinert chiral separations in pharmaceutical, bioanalytical and metabolomics applications.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100347"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148167205","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}
{"title":"Leveraging the potential of capsule phase microextraction for simultaneous determination of anaesthetic and opioid drugs in postmortem samples of its fatal intoxication","authors":"Bharti Jain , Rajeev Jain , Abuzar Kabir , Torki Zughaibi , Shweta Sharma","doi":"10.1016/j.jcoa.2025.100291","DOIUrl":"10.1016/j.jcoa.2025.100291","url":null,"abstract":"<div><div>The reliable identification of anaesthetic and opioid drugs in biological matrices is of critical importance in forensic toxicology, particularly in cases of drug misuse and suspected medical malpractice. Given the typically low concentrations of these analytes in postmortem samples, an efficient extraction and preconcentration strategy is indispensable. Capsule phase microextraction (CPME), a recently developed sol-gel–based sample preparation technology that encapsulates sorbents within a porous tubular polymeric membrane, was employed for the selective isolation of anaesthetics (bupivacaine, lidocaine, ropivacaine, and prilocaine) and the opioid (tramadol) from postmortem blood and tissue samples (liver, kidney, stomach, and spleen). Subsequent analysis was performed using gas chromatography–mass spectrometry (GC–MS). The optimized CPME-GC–MS method exhibited excellent analytical performance, achieving linear calibration ranges of 0.01–1.0 μg mL⁻¹ in blood and 0.01–1.0 μg g⁻¹ in tissue samples, with limits of quantification as low as 0.0060–0.0079 μg mL⁻¹ (blood) and 0.0080–0.0099 μg g⁻¹ (tissues). Precision studies confirmed strong method reliability, with intra-day repeatability below 5% and inter-day reproducibility below 10%. The method was successfully applied to authentic postmortem specimens from a suspected fatal intoxication case attributed to medical negligence involving anaesthetic and opioid drugs. Beyond its forensic applicability, the environmental and operational sustainability of the protocol was critically evaluated using ComplexMoGAPI, AGREE and CACI assessment tools, confirming the method’s greenness and practicality. Overall, the CPME-GC- MS workflow offers a robust, sensitive, and eco-friendly analytical platform, representing a significant advancement for drug monitoring in medico-legal investigations.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100291"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145618377","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}
{"title":"Water and organic content tuning of mobile phase for Enantioseparation of fungicides by capillary electrochromatography using cellulose Tris(3‑chloro-4-methylphenylcarbamate) based stationary phase","authors":"Giovanni D’Orazio , Salvatore Fanali","doi":"10.1016/j.jcoa.2025.100289","DOIUrl":"10.1016/j.jcoa.2025.100289","url":null,"abstract":"<div><div>This study investigated the effect of mobile phase composition, especially water content in a mixture of protic and non-protic organic solvents, on chiral recognition and separation efficiency using a cellulose tris(3‑chloro-4-methylphenylcarbamate)-based stationary phase in the enantioseparation of selected fungicide compounds. The chiral stationary phase, coated on porous native silica particles, was packed into fused silica capillaries (250 mm x 100 µm I.D.) via the \"slurry\" packing method. The capillary column was utilized for the enantiomeric separation of five azole compounds through capillary electrochromatography. The primary objective was to thoroughly investigate how the composition of the mobile phase affects enantioresolution. This was achieved by systematically varying the ratios of methanol, acetonitrile, and water while keeping the buffer concentration, type, and pH constant. The role of water content was studied in relation to chiral interactions by evaluating its effect on key chromatographic parameters such as retention factor, resolution, and efficiency.</div><div>By selecting an appropriate acetonitrile to methanol ratio at a fixed water content, chiral resolutions (<em>Rs</em>) ranging from approximately 2.0 to 3.5 were achieved for the tested analytes.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100289"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145618379","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}
Maria Chiara Frondaroli, Edoardo Parisi, Vittoria Terrigno, Erica Cutè, Susanna Della Posta, Chiara Fanali
{"title":"Recent advances in gels application for green analytical sample preparation","authors":"Maria Chiara Frondaroli, Edoardo Parisi, Vittoria Terrigno, Erica Cutè, Susanna Della Posta, Chiara Fanali","doi":"10.1016/j.jcoa.2026.100311","DOIUrl":"10.1016/j.jcoa.2026.100311","url":null,"abstract":"<div><div>The ongoing quest for more environmentally sustainable analytical methodologies has led to the development of gels as highly versatile and promising materials for sample preparation. Their high surface area, adjustable porosity, mechanical stability, and the capacity to accommodate a diverse array of functional chemical groups, render them remarkably well-suited for the selective capture, retention, and regulated release of a broad spectrum of analytes. Recent studies have demonstrated significant advancements in the field of gel research and innovation, including hydrogels, ionogels, eutectogels, xerogels, aerogels, and cryogels. It has been demonstrated that the properties of gels can be modulated for a variety of sample preparation techniques, including solid-phase extraction, dispersive SPE, magnetic SPE, solid-phase microextraction, and matrix solid-phase dispersion. The synergy between gels and nanostructured materials, such as metal–organic frameworks, carbon nanotubes, graphene oxide, and magnetic nanoparticles, and many others, leads to a pronounced increase in extraction capacity and selectivity. Thus, gel-based materials are gaining attention over a wide range of analytical purposes, including environmental monitoring, food safety testing, and biological analysis.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100311"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146172915","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}
Sanka N. Atapattu , Anurag S. Rathore , Salvatore Fanali
{"title":"Editorial on “Recent Advances in Bioanalysis” virtual special issue","authors":"Sanka N. Atapattu , Anurag S. Rathore , Salvatore Fanali","doi":"10.1016/j.jcoa.2026.100336","DOIUrl":"10.1016/j.jcoa.2026.100336","url":null,"abstract":"","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100336"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148231046","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}
Giulia Giacoppo , Charlotte Mase , Marco Piparo , Pierre Giusti , Caroline Mangote , Callum Branfoot , Luisa Pasti , Flavio Antonio Franchina , Marco Beccaria
{"title":"Preliminary characterization of wind turbine blade waste by solvolysis, microwave-assisted extraction, and comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry","authors":"Giulia Giacoppo , Charlotte Mase , Marco Piparo , Pierre Giusti , Caroline Mangote , Callum Branfoot , Luisa Pasti , Flavio Antonio Franchina , Marco Beccaria","doi":"10.1016/j.jcoa.2025.100301","DOIUrl":"10.1016/j.jcoa.2025.100301","url":null,"abstract":"<div><div>The growth of renewable energy infrastructure highlights the urgent need for sustainable solutions to manage its end-of-life materials, including wind turbine blades (WTBs). These composite materials present significant challenges in recycling due to their complex heterogeneous structure and varied chemical composition. To depolymerize WTB composite materials, a solvolysis process was applied. The resulting chemical products underwent microwave-assisted extraction (MAE), using a mixture of <em>n-</em>hexane and methanol (10:3, v:v). The non-polar organic phase was subjected to analysis using comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry (GC×GC-ToFMS). On the basis of electron impact ionization mass spectral matching at 70 eV, linear retention index data, and molecular distribution on the two-dimensional space, >110 compounds were putatively identified, mainly composed by aromatic and heteroatom-containing species. To the best of our knowledge, this is the first time that the molecular composition of WTBs has been investigated by MAE-GC×GC–MS.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100301"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145789691","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}
{"title":"Surrogate chromatographic models and the solvation parameter model","authors":"Sanka N. Atapattu , Colin F. Poole","doi":"10.1016/j.jcoa.2025.100292","DOIUrl":"10.1016/j.jcoa.2025.100292","url":null,"abstract":"<div><div>Many partition processes of interest have been characterised using Abraham's solvation parameter model. However, to estimate physicochemical, environmental, or biophysical properties of compounds requires reliable solute descriptors. Exploitation of the correlation of partition processes and chromatographic retention data is an alternative approach to estimate properties of interest without relying on solute descriptors. The system constants of the solvation parameter model, along with screening tools such as Cos θ, <em>d</em>-parameter, <em>D</em>-parameter, principal component analysis, and hierarchical cluster analysis, facilitate the identification of similarities between partitioning and chromatographic systems. In this review we discuss various screening tools to identify similarities between partitioning and chromatographic systems as well as applications of surrogate chromatographic models to estimate physicochemical, environmental, and biophysical properties of interest.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100292"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145618381","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}
Özge Cansın Zeki , Fatma Ilgaz , Cemil Can Eylem , Selin Seda Timur , Hakan Eroğlu , Hülya Gökmen-Özel , Emirhan Nemutlu
{"title":"Gas chromatography mass spectrometry based pharmacometabolomic assessment of formulation-dependent metabolic responses of levetiracetam","authors":"Özge Cansın Zeki , Fatma Ilgaz , Cemil Can Eylem , Selin Seda Timur , Hakan Eroğlu , Hülya Gökmen-Özel , Emirhan Nemutlu","doi":"10.1016/j.jcoa.2026.100315","DOIUrl":"10.1016/j.jcoa.2026.100315","url":null,"abstract":"<div><div>This study applied a GC–MS–based pharmacometabolomic approach to investigate formulation-dependent bioavailability and systemic metabolic responses following levetiracetam administration. Plasma samples from rabbits were analyzed after receiving three different formulations: a control formulation in which levetiracetam was mixed with deionized water, a Multithick formulation prepared with an 8% modified maize starch thickener, and a Thicken-Up Clear (TUC) formulation prepared with 3.6% xanthan gum thickener. Although dissolution profiles varied substantially among these formulations, likewise, total levetiracetam exposure, represented by AUC, did not differ significantly among groups (<em>p</em> < 0.05). Untargeted GC–MS analysis was annotated 97 metabolites and multivariate analysis revealed distinct metabolic clustering, with the TUC group showing the most pronounced separation. Correlation analysis identified five metabolites that were positively associated with pharmacokinetic parameters: pyrophosphate, glyceric acid, aconitic acid, methyl-2-butenedioic acid, and itaconic acid. Six amino acid–related metabolites showed negative associations, reflecting enhanced energy metabolism together with reduced excitatory neurotransmission, consistent with the known neuroprotective and antiepileptic actions of levetiracetam. Overall, these results demonstrate that formulation design influences not only dissolution behavior but also systemic metabolic responses. Pharmacometabolomics offers a quantitative framework for integrating chromatographic, pharmacokinetic and biochemical data to support rational formulation development and precision pharmacotherapy.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100315"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147384202","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}
{"title":"A sustainable approach to the identification of plant matrices by nano-liquid chromatography and nuclear magnetic resonance spectroscopy: Artichoke leaves sample","authors":"A.P. Sobolev , C. Dal Bosco , G. D’Orazio","doi":"10.1016/j.jcoa.2026.100342","DOIUrl":"10.1016/j.jcoa.2026.100342","url":null,"abstract":"<div><div>The phytochemical characterization of vegetable matrices is a key aspect of modern analytical chemistry, driven by the growing interest in plant-based nutraceuticals. However, traditional lipophilic extraction methods often rely on toxic solvents like chloroform, which conflicts with the principles of Green Analytical Chemistry (GAC). This study presents a sustainable analytical workflow for the identification of both hydrophobic primary and secondary metabolites in artichoke (<em>Cynara cardunculus</em> var. <em>scolymus</em>) leaves. A comparison of traditional chloroform extraction with environmentally friendly alternatives, including anisole, ethyl acetate, and isoamyl acetate, was examined. Additionally, an hydrophobic Natural Deep Eutectic Solvent (NaDES) was used to evaluate its extraction efficiency. The extracts were analyzed using both a miniaturized technique, such as nano-liquid chromatography (nano-LC), and nuclear magnetic resonance (NMR) spectroscopy to identify and semi-quantify fatty acids, lipids, sterols, and, in particular, sesquiterpene lactones (STLs), such as cynaropicrin. The results show that bio-based solvents, especially isoamyl acetate and anisole, offer a practical and sustainable alternative for extracting lipophilic compounds, aligning the process with GAC principles. Theoretical assessments using Hansen Solubility Parameters (HSP), <em>LogP</em>, and surface tension confirmed that these green substitutes can effectively replace chloroform. Specifically, the balance between thermodynamic affinity and mass-transfer kinetics ensured high recovery rates for STLs, demonstrating that both high qualitative extraction profile and quantitative recovery can be preserved in a fully sustainable workflow. Finally, the AgreePrep metric was applied to compare the sustainability of the sample preparation using chloroform and the most promising alternative solvent for the future development of a quantitative method.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100342"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147950876","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}
Barbara Sechi , Giorgi Jibuti , Roberto Dallocchio , Sergio Cossu , Bezhan Chankvetadze , Victor Mamane , Paola Peluso
{"title":"Erratum to “On the effect of aqueous organic mobile phases on the enantioseparation of halogenated 4,4’-bipyridines using polysaccharide carbamate-based chiral columns” [Journal of Chromatography Open Volume 9 (2026) 100319]","authors":"Barbara Sechi , Giorgi Jibuti , Roberto Dallocchio , Sergio Cossu , Bezhan Chankvetadze , Victor Mamane , Paola Peluso","doi":"10.1016/j.jcoa.2026.100329","DOIUrl":"10.1016/j.jcoa.2026.100329","url":null,"abstract":"","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"9 ","pages":"Article 100329"},"PeriodicalIF":3.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148231042","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}