{"title":"Simultaneous analysis of sulfolane and BTEX in rock samples by gas chromatography–mass spectrometry","authors":"Merrik Kobarfard , Jennie Hansson , Beth Parker , Tadeusz Górecki","doi":"10.1016/j.jcoa.2025.100264","DOIUrl":"10.1016/j.jcoa.2025.100264","url":null,"abstract":"<div><div>Sulfolane is a water-miscible industrial solvent that has been widely utilized in various industries. Once released into the environment, it can infiltrate fractured rock structures in groundwater zones, leading to long-term contamination. Benzene, toluene, ethylbenzene, and xylenes (collectively known as BTEX) are commonly associated with sulfolane in the petrochemical industry. The presence and mobility of sulfolane can influence the distribution and transport behavior of BTEX at contaminated sites. Therefore, simultaneous analysis and monitoring of these compounds are crucial for understanding the source and fate of contamination.</div><div>In this study, a gas chromatography-mass spectrometry (GC–MS) method was developed and validated for the simultaneous quantitation of sulfolane and BTEX in rock samples. To address the slow release of sulfolane observed in certain samples when left in methanol and to facilitate rapid analysis, a microwave-assisted extraction (MAE) method was optimized for sample preparation. Analysis of spiked samples yielded recoveries of 86 % to 115 % for the various analytes, with relative standard deviations of up to 7.9 %. The validated method was then applied to rock samples collected from a contaminated site in central Alberta, Canada. All analyzed samples were contaminated with toluene. Only one sample was found to be contaminated with sulfolane. Ethylbenzene, <em>o-</em>xylene, <em>m</em>/<em>p-</em>xylene and benzene were detected in 82 %, 44 %, 40 %, and 4 % of the samples, respectively. Although the concentrations of these contaminants were all below the Alberta Tier 1 Soil Remediation Guidelines, the sampling covered only a limited depth. Therefore, additional sampling and investigation are necessary to conclusively determine the status of persistent contamination at the site.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100264"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145219109","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":"Advancements in molecularly imprinted polymers-based monolithic structures for biomedical analysis","authors":"Özge Altıntaş , Fatma Yılmaz , Adil Denizli","doi":"10.1016/j.jcoa.2025.100255","DOIUrl":"10.1016/j.jcoa.2025.100255","url":null,"abstract":"<div><div>Molecularly imprinted polymers (MIPs) have emerged as a promising alternative in biomedical analysis due to their specific recognition capabilities, chemical stability and applicability in biological systems. This review focuses on recent advancements in MIP systems those integrated with monolithic structures for biomedical analytical applications. Owing to their high surface area, low flow resistance and porous morphology, monolithic MIPs exhibit superior performance in applications such as separation, diagnostics and targeted drug delivery. Compared to conventional particle-based systems, these structures are more readily integrated into microfluidic platforms and yield more effective outcomes in sample preparation, sensor-based diagnostics and chromatographic separations. Moreover, novel technologies such as 3D printing and stimuli-responsive materials further enhance the functionality of these polymers, facilitating their translation into future clinical applications. This review systematically discusses the design, synthesis strategies, analytical performance and biomedical potential of MIP-monolith composites. By considering existing challenges, it also highlights their potential for developing of high-performance systems with broader application scopes in the future.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100255"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145018626","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}
Cemil Aydoğan , Zeynep Günyel , Ashraf Ali , Ilgım Göktürk , Fatma Yılmaz , Adil Denizli
{"title":"Recent advances and applications of miniaturized analytical- and on-line sample preparation- columns","authors":"Cemil Aydoğan , Zeynep Günyel , Ashraf Ali , Ilgım Göktürk , Fatma Yılmaz , Adil Denizli","doi":"10.1016/j.jcoa.2025.100247","DOIUrl":"10.1016/j.jcoa.2025.100247","url":null,"abstract":"<div><div>Miniaturized columns are chromatographic columns used in modern LC applications, which are in narrow diameter format while CE/CEC separations with miniaturized columns show high separation efficiency due to flat flow profile from EOF. There are several variants of miniaturized columns with both analytical- and trap columns. This review summarizes and discusses recent advances and applications on miniaturized analytical- and on-line sample preparation- columns focussing on literature mostly between 2019 and 2024.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100247"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144866481","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":"Optimization of immobilized metal affinity chromatography for a recombinant protein expressed in CHO cells","authors":"Xiaoyong Jiang , Rongqiu Qin , Tengfei Ma, Kexin Xu, Fengjuan Lv","doi":"10.1016/j.jcoa.2025.100230","DOIUrl":"10.1016/j.jcoa.2025.100230","url":null,"abstract":"<div><div>Immobilized metal affinity chromatography (IMAC) is widely used in research laboratories to purify His-tagged proteins expressed in Escherichia coli (<em>E. coli</em>) by enabling direct capture and moderate removal of process-related impurities, such as host cell proteins (HCPs) and DNA. However, its application for purifying recombinant proteins secreted by mammalian cells is limited due to incompatibility issues between cell culture media and IMAC resins. In this study, we purified a CHO-expressed and secreted recombinant protein with His-tag using a Ni Sepharose excel resin, resistant to EDTA and reducing agents, and optimized loading, washing, and elution conditions to maximize protein recovery and HCP clearance. The resin demonstrated a maximum load capacity of 10 mg/mL. Results show that incorporating Triton X-100, PS80 & TnBP, or 2-propanol in washing buffers significantly improves HCP removal while maintaining low salt concentrations in the elution buffer enhances both yield and product quality. Resin lifetime studies conducted under optimal conditions showed acceptable yields, stable product quality attributes (PQAs), and effective cleaning over 54 purification cycles. This protocol provides a robust IMAC purification strategy, potentially broadening its industrial applications.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100230"},"PeriodicalIF":0.0,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144272210","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":"Comment on ‘From multimodal liquid chromatography to supercritical fluid chromatography: Mapping chiral separation of the major organic ultraviolet filters’ (JCO 8 (2025) 100251. https://doi.org/10.1016/j.jcoa.2025.100251) - peak assignment for cis- and trans-homosalate","authors":"Daniel Bury, Katharina E. Ebert, Holger M. Koch","doi":"10.1016/j.jcoa.2025.100277","DOIUrl":"10.1016/j.jcoa.2025.100277","url":null,"abstract":"","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100277"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145473913","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}
Paula Albendea, Aleksandra Gorska, Giorgia Purcaro
{"title":"Optimization of a miniaturized microwave-assisted saponification and extraction method to evaluate mosh and MOAH in biological samples","authors":"Paula Albendea, Aleksandra Gorska, Giorgia Purcaro","doi":"10.1016/j.jcoa.2025.100267","DOIUrl":"10.1016/j.jcoa.2025.100267","url":null,"abstract":"<div><div>Mineral oil hydrocarbons (MOH) are a group of lipophilic contaminants composed of thousands of different compounds. The human toxicokinetics (absorption, metabolization, distribution and elimination) of these contaminants depends on their molecular structure but information are still lacking. The primary gap to be filled is the optimization and validation of a method to treat a very small amount of samples, as the ones produced during in-vitro studies.</div><div>The aim of this study is to develop and validate a miniaturized microwave-assisted saponification and extraction (MASE) method for the evaluation of MOH subclasses in low amounts of biological samples (<400 mg). The method was validated using an LC/GC×GC-FID/MS system in mono- and two-dimensional modes. The results demonstrated excellent recovery (≥94 %), repeatability, and compliance with JRC (Joint Research Center) guidance criteria for internal standard ratios. Furthermore, the method achieved a limit of quantification as low as 0.4 µg of MOH in the sample, outperforming conventional extraction methods.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100267"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145265454","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}
Tuğçe Öztepe, Cemil Can Eylem, Tuba Reçber, Emirhan Nemutlu
{"title":"Advances in dual-column chromatography for metabolomics: Opportunities, challenges, and applications","authors":"Tuğçe Öztepe, Cemil Can Eylem, Tuba Reçber, Emirhan Nemutlu","doi":"10.1016/j.jcoa.2025.100266","DOIUrl":"10.1016/j.jcoa.2025.100266","url":null,"abstract":"<div><div>Metabolomics, a dynamic and rapidly evolving omics discipline, provides critical insights into the biochemical state of biological systems and holds transformative potential in fields such as biomarker discovery, disease mechanisms, and precision medicine. As the demand for high-throughput, unbiased, and reproducible metabolite profiling grows, particularly in clinical and translational settings, there is an urgent need for analytical platforms that can simultaneously address chemical diversity, sensitivity, and standardization.</div><div>Traditional single-column chromatographic systems often fall short in capturing the full spectrum of metabolites due to limited polarity range and separation capacity, leading to analytical blind spots and suboptimal data integration. In response to these limitations, dual-column systems have emerged as a promising solution by integrating orthogonal separation chemistries (e.g., reversed-phase; RP and hydrophilic interaction chromatography; HILIC) within a single analytical workflow. These systems offer superior performance by enabling the concurrent analysis of both polar and nonpolar metabolites, thereby reducing analysis time, improving sensitivity, and enhancing coverage, particularly in hybrid designs that unify targeted and untargeted metabolomics approaches.</div><div>However, despite their growing adoption, a comprehensive assessment of dual-column platforms, including design, performance, and advantages for metabolomics applications, remains limited. This review addresses this gap by systematically covering dual-column LC-MS applications in metabolomics reported between 1984 and 2025, comparing targeted and untargeted approaches and evaluating platform configurations, analytical capabilities, and contributions to workflow standardization. Furthermore, by discussing key methodological aspects, such as sample preparation, column setup, detection strategies, and data analysis, we highlight how these systems impact data quality and facilitate robust biological interpretation.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100266"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145324679","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}
Erika Maria Ricci , Enrico Dainese , Vincenzo De Laurenzi , Giulio Lovato , Gianluca Sala , Marcello Locatelli , Miryam Perrucci
{"title":"New analytical challenges in characterization of antibody-drug conjugates","authors":"Erika Maria Ricci , Enrico Dainese , Vincenzo De Laurenzi , Giulio Lovato , Gianluca Sala , Marcello Locatelli , Miryam Perrucci","doi":"10.1016/j.jcoa.2025.100260","DOIUrl":"10.1016/j.jcoa.2025.100260","url":null,"abstract":"<div><div>Since 1913, when Paul Ehrlich introduced the concept of “selective toxicity”, new strategies to obtain quality control, quantification of the drug were mandatory. For this reason, the introduction of antibody drug conjugates (ADC) has shown many critical points, being these systems made of small- and high-molecular weight compounds. Being ADCs a novelty for showing therapeutic action, they were subjected to a grow up in studies. There are in literature several approaches to follow ADCs for <em>in vivo</em> and <em>in vitro</em> studies because type of conjugation, release of the drug, and body-distribution are characteristic for each of them, resulting in many critical steps.</div><div>Liquid chromatography (LC) and capillary electrophoresis (CE) are the most common analytical technique used in order to obtain the aim. For the characterization of ADCs, there are several chromatographic techniques. HPLC finds application in both small and large molecules, related to the availability of various modes of separation (reversed-phase, size exclusion, ion exchange, mixed-mode etc.). Capillary electrophoresis (CE) finds its main application in large molecule therapeutics, where its electrophoretic separation mechanism offers a distinct, and often superior, separation of macromolecules compared to classic chromatographic techniques. Several modes of CE, including capillary electrophoresis sodium dodecyl sulphate (CE-SDS), capillary zone electrophoresis (CZE), and capillary isoelectric focusing (CIEF) or imaged capillary isoelectric focusing (iCIEF) are commonly utilized in characterization of the critical quality attributes (CQAs) of monoclonal antibody drugs such as charge variants, size variants, and positional isomers/purity etc.</div><div>In this review, analytical methods for physicochemical characterization of ADCs will be reported and analysed in order to highlight as the chromatographic procedures allow obtaining a complete ADCs evaluation and characterization.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100260"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145158055","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}
Miryam Perrucci , Imran Ali , Fotouh R. Mansour , Halil I. Ulusoy , Songül Ulusoy , Abuzar Kabir , Ornella Abollino , Agnese Giacomino , Paolo Inaudi , Marcello Locatelli , Erika Maria Ricci
{"title":"Chemical analysis using miniaturized and Portable 3D printed systems: Where are we now?","authors":"Miryam Perrucci , Imran Ali , Fotouh R. Mansour , Halil I. Ulusoy , Songül Ulusoy , Abuzar Kabir , Ornella Abollino , Agnese Giacomino , Paolo Inaudi , Marcello Locatelli , Erika Maria Ricci","doi":"10.1016/j.jcoa.2025.100241","DOIUrl":"10.1016/j.jcoa.2025.100241","url":null,"abstract":"<div><div>With the growing emphasis on green chemistry (GC) and green analytical chemistry (GAC), significant efforts have been directed toward minimizing sample size and simplifying sample preparation procedures. Concurrently, ongoing research has enabled the miniaturization of instrumental configurations used for quantitative analysis, aligning with the principles of sustainability.</div><div>One major challenge lies in the inherent complexity of liquid chromatography systems, which comprise multiple interconnected components. Each component has been subject to miniaturization, with careful attention to preserving analytical sensitivity, selectivity, and accuracy when applied to real samples. Interest in miniaturized systems is further fueled by the theoretical principle that reducing flow rates enhances the surface-to-volume ratio, thereby improving detection sensitivity.</div><div>Building on this theoretical foundation—particularly the goals of portability, efficient sampling, and <em>on site</em> analysis—innovative approaches such as microfluidics and 3D printing have been employed to develop compact fluidic systems. These technologies not only broaden the scope of liquid chromatography but also open new frontiers, such as drug testing on engineered tissues, and the development of new devices suitable for space missions.</div><div>This review aims to present a comprehensive overview of the challenges encountered and the advancements achieved in the miniaturization of instrumental setups and portable systems, encompassing both pre- and post-analytical stages. Furthermore, a discussion on 3D technologies available for LC-chip and miniaturized systems was also presented.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100241"},"PeriodicalIF":0.0,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144633153","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}
Cristina Grazia De Nido , Diego Centonze , Carmen Palermo , Javier González-Sálamo , Javier Hernández-Borges
{"title":"Microplastics in salt: A critical review of contamination, analytical methodologies, and health implications","authors":"Cristina Grazia De Nido , Diego Centonze , Carmen Palermo , Javier González-Sálamo , Javier Hernández-Borges","doi":"10.1016/j.jcoa.2025.100276","DOIUrl":"10.1016/j.jcoa.2025.100276","url":null,"abstract":"<div><div>Microplastic pollution has emerged as a growing environmental concern due to the rapid and widespread distribution of these particles, their entry into the food chain, and their potential implications for human health. Among food products, salt has gained attention as a relevant indicator of microplastic contamination, given its widespread consumption and direct environmental exposure during production. This review provides a comprehensive overview of current knowledge on the occurrence of microplastics in commercial salt, with a particular focus on sample pretreatment protocols, analytical techniques employed, and the diverse morphotypes in which microplastics are found, factors that are critical for accurate identification and quantification. Although research in this field is still evolving, existing studies offer valuable insights into the extent of contamination and serve as useful tools for environmental monitoring. Using salt as a model matrix, this review also reflects on the broader dietary and ecological implications of microplastic pollution, highlighting the need for improved methodologies and sustainable strategies to mitigate this emerging threat.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100276"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145416040","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}