A. Temerdashev , S. Girel , S.N. Atapattu , Y.-Q. Feng , E. Gashimova , T. Malitskaya , I. Podolskiy , Q.-F. Zhu
{"title":"Liquid chromatography coupled to mass spectrometry for steroid hormones analysis: issues and solutions in sample preparation and method development","authors":"A. Temerdashev , S. Girel , S.N. Atapattu , Y.-Q. Feng , E. Gashimova , T. Malitskaya , I. Podolskiy , Q.-F. Zhu","doi":"10.1016/j.jcoa.2025.100250","DOIUrl":"10.1016/j.jcoa.2025.100250","url":null,"abstract":"<div><div>Current work presents main aspects of the application of liquid chromatography in combination with low- and high-resolution mass spectrometry to an analysis of steroid hormones. Advantages and challenges of both targeted and untargeted analysis are shown together with the most popular approaches to the associated sample preparation. Among emerging approaches, first applications of isotope ratio mass spectrometry in combination with liquid chromatography for the analysis of steroid hormones for doping control purposes are presented and discussed.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100250"},"PeriodicalIF":3.2,"publicationDate":"2025-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145049340","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":"2025-09-04","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}
{"title":"Nanotechnology in bioanalysis: Current trends and applications","authors":"Arshdeep Chopra , Yogindra Kumari , Samarth Kumar , Renuka Sharma , 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":"2025-09-03","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}
Abdul Haseeb , Yosief Wondmagegne , Miguel X. Fernandes , Jörgen Samuelsson
{"title":"Adsorption energy distributions: Theory and applications in liquid chromatography","authors":"Abdul Haseeb , Yosief Wondmagegne , Miguel X. Fernandes , 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":"2025-09-02","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}
Leandro Oka-Duarte , Giovanni S. Baviera , Weston J. Umstead , Quezia B. Cass , Anderson R.M. de Oliveira
{"title":"From multimodal liquid chromatography to supercritical fluid chromatography: Mapping chiral separation of the major organic ultraviolet filters","authors":"Leandro Oka-Duarte , Giovanni S. Baviera , Weston J. Umstead , Quezia B. Cass , Anderson R.M. de Oliveira","doi":"10.1016/j.jcoa.2025.100251","DOIUrl":"10.1016/j.jcoa.2025.100251","url":null,"abstract":"<div><div>The widespread presence of chiral organic UV filters in the environment raises critical concerns due to their potential enantioselective toxicity and persistence. This study provides the first comprehensive enantioseparation screening of five such compounds – enzacamene, homosalate, octinoxate, octisalate, and octocrylene – using multimodal liquid chromatography (LC), as well as supercritical fluid chromatography (SFC) with 20 polysaccharide-based chiral stationary phases (CSPs). Enzacamene and homosalate were baseline-resolved across all tested conditions, including SFC, while octisalate showed separation in normal and reversed-phase modes. Octinoxate was resolved only in normal-phase mode, and octocrylene was not fully resolved, though near-baseline separation was achieved in polar organic and normal-phase modes. SFC, particularly with non-conventional CO₂/hexane–ethanol eluent, proved complementary to LC, achieving comparable or superior enantioresolution. Coated amylose columns demonstrated superior performance in reversed-phase mode, whereas immobilized CSPs, particularly chloromethylphenylcarbamate-based selectors, displayed broader applicability across multiple mobile phase systems. These findings emphasize the necessity of multimodal approaches to optimize the enantioseparation of highly lipophilic environmental contaminants and establish a robust analytical foundation for future ecotoxicological and regulatory studies.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100251"},"PeriodicalIF":3.2,"publicationDate":"2025-09-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145010209","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}
Rachel C. Halvorsen , Wenjing Ma , Caitlin N. Cain , Hep Ingham , Rachel E. Mohler , Robert E. Synovec
{"title":"Implementing tile-based fisher ratio analysis of two-dimensional gas chromatography time-of-flight mass spectrometry data to obtain a master peak table of all detected analyte compounds in many petroleum-based samples","authors":"Rachel C. Halvorsen , Wenjing Ma , Caitlin N. Cain , Hep Ingham , Rachel E. Mohler , Robert E. Synovec","doi":"10.1016/j.jcoa.2025.100249","DOIUrl":"10.1016/j.jcoa.2025.100249","url":null,"abstract":"<div><div>Historically, tile-based Fisher ratio (F-ratio) analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) data was developed for analysts to use a supervised experimental design with defined sample classes to obtain a hit list to discover analytes that most significantly distinguish the sample classes at the top of the hit list. In this traditional application, a user-specified F-ratio threshold is used to discard most hits in order to focus on the top hits. To broaden the scope of tile-based F-ratio analysis, in the present study we explore the ability of the software to discover all analyte components that are detected in a set of samples, essentially taking full advantage of the tiling aspect of the software which uncovers all analytes that exhibit sufficient signal relative to the baseline noise across all samples to be deemed detectable and hence to produce an F-ratio. For this study a set of nine petroleum samples, i.e., two hydrobates (light naphthas), two reformates, four naphthas, and a “heavy” gasoline, are simultaneously analyzed and statistically compared via p-testing to blank chromatograms to produce one comprehensive hit list. The pin locations and signal areas at the top <em>m/z</em> F-ratio are used together with replicate blanks to generate a master peak table (MPT) that in turn is used to generate sample-specific peak tables (SSPT), one SSPT for each injection replicate of each petroleum sample (class), that are naturally retention-time aligned via the F-ratio software. The nine petroleum samples vary to a large extent in the identity and number of analytes present. Indeed, while a total of ∼715 analytes were found across all nine samples, only ∼260 of these analytes are fully shared across all sample classes. The number of analytes in the nine petroleum samples ranged from an average of 335 analytes for one of the hydrobates to 669 analytes for two of the naphthas. This workflow also facilitated generating simulated distillation curves for the nine petroleum samples to provide further insight.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100249"},"PeriodicalIF":3.2,"publicationDate":"2025-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145004276","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}
Janik D. Seidel , Clifford Young , Manuela Klingler-Hoffmann , Mark R. Condina , Alok Shah , Sri Ramarathinam , Woan Mei Kok , Craig Kyngdon , Peter Hoffmann
{"title":"Analytical methods for in-depth characterisation of cell culture bioreactors: A case study","authors":"Janik D. Seidel , Clifford Young , Manuela Klingler-Hoffmann , Mark R. Condina , Alok Shah , Sri Ramarathinam , Woan Mei Kok , Craig Kyngdon , Peter Hoffmann","doi":"10.1016/j.jcoa.2025.100248","DOIUrl":"10.1016/j.jcoa.2025.100248","url":null,"abstract":"<div><div>Biopharmaceuticals and especially antibodies represent an expanding segment of pharmaceutical drug products. Production processes for this group of complex molecules use biological expression systems such as Chinese hamster ovary (CHO) cells, that are instrumental in their assembly, folding, and post-translational modification. Process development and optimization is challenging due to the complexity of cell culture systems and interdependency of process parameters on product quality attributes. This case study presents newly applied and developed analytical technologies able to monitor the cell culture process to increase the understanding of the interconnection of process parameters and quality attribute relationships in biopharmaceutical production processes. Specifically, a high-performance liquid chromatography (HPLC) -based workflow routinely measures amino acids and other cell culture media component profiles, while a mass spectrometry-based workflow monitors and quantifies changes in expressions of host cell proteins (HCPs) both globally and for individual HCP during the culture duration. These methods were applied to an industrial process with variations in seeding density, glucose and media feeding strategy, and media composition. Observations on product titre, global HCP and individual high-risk HCPs, throughout the culture progress, as well as in the end of the culture, provide insight for potential further optimization.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100248"},"PeriodicalIF":3.2,"publicationDate":"2025-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144892109","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":"Integrating ultrashort-chain compounds into the comprehensive analysis of per- and polyfluorinated substances in ready-to-feed liquid milk samples","authors":"Shun-Hsin Liang, 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":"2025-08-14","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}
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":"2025-08-14","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}
Allan Polidoro , Valentina Costa , Monica Romagnoli , Elena Sarti , Claudia Stevanin , Cinzia Fabbro , Luisa Pasti , Flavio A. Franchina
{"title":"Multitargeted analysis for the simultaneous determination of organochlorine pesticides and polychlorinated biphenyls in sediments exploiting comprehensive two-dimensional gas chromatography coupled to mass spectrometry","authors":"Allan Polidoro , Valentina Costa , Monica Romagnoli , Elena Sarti , Claudia Stevanin , Cinzia Fabbro , Luisa Pasti , Flavio A. Franchina","doi":"10.1016/j.jcoa.2025.100245","DOIUrl":"10.1016/j.jcoa.2025.100245","url":null,"abstract":"<div><div>Persistent organic pollutants (POPs), including organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs), remain a significant environmental concern due to their persistence, bioaccumulation, and toxicity. Accurate quantification of these contaminants in sediment matrices remains analytically challenging due to the complexity of the matrix and the need for detection at trace levels to meet regulatory standards. This research focused on the development and application of an analytical protocol for the simultaneous determination of OCPs and PCBs in sediments using solid-phase extraction (SPE) followed by comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS). The developed method was validated, achieving low limits of detection (0.4 to 14 ng kg<sup>-1</sup>) and quantification (1.1 to 41 ng kg<sup>-1</sup>), with satisfactory linearity (r² > 0.99), accuracy (90–110%), and precision (RSD < 5%) for all target analytes. Validation with certified reference material confirmed the agreement between experimental and certified concentrations for most compounds. The protocol was applied to environmental sediment samples, detecting multiple PCBs and DDT-related compounds at concentrations below international guideline values. These results confirm the method’s suitability for trace-level determination of OCPs and PCBs in sediments, addressing the analytical demands of environmental monitoring and regulatory compliance. The established protocol enables sensitive and reliable assessment of sediment contamination, supporting a simultaneous ongoing surveillance and risk assessment of such classes of persistent organic pollutants in the same analytical run.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100245"},"PeriodicalIF":3.2,"publicationDate":"2025-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144842201","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}