Journal of chromatography open最新文献

{"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 ,&nbsp;Wenjing Ma ,&nbsp;Caitlin N. Cain ,&nbsp;Hep Ingham ,&nbsp;Rachel E. Mohler ,&nbsp;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":"2025-11-01","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}

{"title":"Enantioselective capillary electrophoresis with sulfated cyclodextrins for monitoring ketamine and its metabolites in biosamples and its application to assess metabolic steps and kinetic parameters","authors":"Wolfgang Thormann","doi":"10.1016/j.jcoa.2025.100256","DOIUrl":"10.1016/j.jcoa.2025.100256","url":null,"abstract":"<div><div>Sulfated cyclodextrin based enantioselective capillary electrophoresis for the monitoring of the stereoisomers of ketamine and its metabolites norketamine, 5,6-dehydronorketamine and hydroxynorketamine in biosamples is reviewed. A survey of reported assays with their specifications is presented together with their limitations in terms of distinguishing between the various hydroxynorketamine stereoisomers formed in vitro and in vivo. Applications discussed include (i) the identification of single cytochrome P450 enzymes that are involved in the various metabolic steps in humans, equines and canines, (ii) the assessment of the metabolic patterns present after incubation of ketamine or norketamine with liver microsomes of different species, (iii) the quantitation of an in vitro metabolic step in absence and presence of an inhibitor, (iv) the monitoring of the stereoisomers of ketamine and its metabolites in urine, plasma, cerebrospinal fluid, brain and hair, and (v) the pharmacokinetics of ketamine and norketamine enantiomers after bolus application, target control infusion or low-dose, subanesthetic constant rate infusion of racemic ketamine and S-ketamine to equines and canines. The reviewed metabolic ketamine work assessed by enantioselective capillary electrophoresis provides insight into the stereoselectivity of the metabolic pathways of ketamine and improved infusion, anesthetic and antinociceptive application schemes of racemic ketamine and S-ketamine in veterinary medicine.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100256"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145049343","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":"Ionic liquids in liquid chromatography","authors":"Sini Santasalo ,&nbsp;Susanne K. Wiedmer","doi":"10.1016/j.jcoa.2025.100239","DOIUrl":"10.1016/j.jcoa.2025.100239","url":null,"abstract":"<div><div>The use of ionic liquids (ILs) in liquid chromatography (LC) is reviewed. ILs have several different types of functionalities, which means that they are prone to multiple simultaneous interactions with stationary phases in LC. ILs have been investigated by LC as analytes and they have been used as mobile phase additives and column stationary phase modifiers in LC. All these applications include a diverse range of interactions with different LC stationary phases. Common reasons for using ILs as mobile phase additives have been to reduce unwanted interactions between analytes and free silanols on the column stationary phase, to act as ion pair reagents to separate polar compounds with reversed phase LC, and to act as UV absorption reagents to detect compounds that do not absorb UV light. The review covers the most important works between 2003–2025.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100239"},"PeriodicalIF":0.0,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144655275","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":"Integrated size- and composition analysis of nanoplastics by hyphenating hydrodynamic chromatography to pyrolysis-gas chromatography-mass spectrometry","authors":"Brian R. van ‘t Veer ,&nbsp;Jasper P.H. Smeets ,&nbsp;Clementina Vitali ,&nbsp;Anna K. Undas ,&nbsp;Sander Affourtit ,&nbsp;Hans-Gerd Janssen","doi":"10.1016/j.jcoa.2025.100261","DOIUrl":"10.1016/j.jcoa.2025.100261","url":null,"abstract":"<div><div>To understand the health impact of micro- and nanoplastics (MNPs), methods to quantify the levels of the various particle size ranges as well as techniques to chemically characterize them are needed. Current analytical strategies largely focus either on the size or the chemical composition of these MNPs, without correlating the two. A novel hyphenated method is presented that combines hydrodynamic chromatography (HDC) with pyrolysis-gas chromatography-mass spectrometry (Py–GC–MS) for integrated size- and composition characterization. Because HDC does not use membranes or stationary phases, the need for mobile phase additives is significantly reduced, simplifying combination with Py–GC–MS identification. In the newly developed method, the effluent of the HDC size separation is fractionated and individual fractions are subjected to Py–GC–MS identification. Introduction of the fractions and subsequent pyrolysis is done using a programmable temperature vaporization (PTV) inlet. The PTV introduction step employs a three-stage temperature program: an initial low-temperature hold for water removal, followed by an additive-removal step at moderate temperature, and finally a treatment at high temperature to pyrolyze the MNPs. The PTV Py–GC–MS method showed a good performance in the analysis of various plastics including PET, PA12, PTFE, PTHF and PE. For other plastics like PAN, PVDC and PVC the identification capability of the method was also good, but quantification was compromised by partial losses of the material during additive removal. Application of the HDC–Py–GC–MS method to a PS nanoplastic mixture, as well as to a representative industrial acrylate/styrene nanoplastic sample, highlighted the method’s potential for correlating size and chemical composition.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100261"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145158054","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":"Quantification of lactate enantiomers in human sweat samples using two-dimensional liquid chromatography","authors":"Kazushi Mori,&nbsp;Makoto Tsunoda","doi":"10.1016/j.jcoa.2025.100243","DOIUrl":"10.1016/j.jcoa.2025.100243","url":null,"abstract":"<div><div>Lactate (LA) is primarily produced by the reduction of pyruvate in the human body and is crucial for energy production via anaerobic glycolysis. Although the D-LA concentration is considerably lower than that of L-LA, a significant increase in D-LA concentration alone has been reported in some diseases. Quantifying LA enantiomers in human biofluids has the potential for disease diagnosis. Sweat has recently been recognized as a novel biological alternative to blood because it can be sampled non-invasively. Therefore, in this study, heart-cutting two-dimensional liquid chromatography (2D-LC) using a highly sensitive fluorescence detection method was developed for the analysis of LA enantiomers in small amounts of human sweat. LA was derivatized with 4-nitro-7-piperazino-2,1,3-benzoxadiazole (NBD-PZ) and separated from endogenous compounds using an octadecyl silica column in the first dimension. Subsequently, the NBD-PZ-LA peak was fractionated and enantiomerically separated in the second dimension on a chiral column. Sufficient linearities (R² &gt; 0.999) were observed in the ranges of 1–100 and 10–1000 µM for NBD-PZ-D-LA and NBD-PZ-L-LA, respectively. The corresponding limits of quantification were 0.97 and 1.12 µM. The precision values were 1.04 %–12.03 %, and the accuracies were 85.6 %–100.4 %. The developed method was successfully applied to ∼5 µL of human sweat collected from five healthy subjects. The concentrations of D-LA and L-LA in sweat were 30.29 ± 20.18 µM and 23.69 ± 12.15 mM, respectively. The developed 2D-LC system should be clinically applicable to LA enantiomer analysis in human sweat as a non-invasive biomarker.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100243"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144738509","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 tutorial on the synthesis and applications of molecularly imprinted polymers in analytical chemistry","authors":"N.P. Kalogiouri ,&nbsp;A. Kabir ,&nbsp;K.G. Furton ,&nbsp;V.F. Samanidou","doi":"10.1016/j.jcoa.2025.100244","DOIUrl":"10.1016/j.jcoa.2025.100244","url":null,"abstract":"<div><div>Molecularly imprinted polymers (MIPs) have emerged as highly selective sorbents with tailor-made recognition sites complementary to target analytes in terms of shape, size, and functional groups. This tutorial provides a comprehensive overview of the principles, synthesis strategies, and analytical applications of MIPs, with a focus on their utility in sample preparation, separation, and detection. Various imprinting techniques—such as bulk, surface, and nanoimprinting—are discussed alongside advances in green synthesis and novel monomer-template systems. Emphasis is placed on the integration of MIPs with chromatographic and spectrometric platforms, particularly in complex matrices relevant to environmental, pharmaceutical, food, and clinical analysis. The tutorial illustrates the practical considerations for designing and optimizing MIP-based methods, including template selection, polymerization conditions, and reusability, reflecting recent and relevant advances of the last ten years This tutorial aims to guide researchers and analysts in leveraging the unique properties of MIPs to enhance selectivity, sensitivity, and sustainability in modern analytical chemistry.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100244"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144750367","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":"Characterization of double bond position in free fatty acids of human sebum","authors":"Alice Telle ,&nbsp;Giulia Mastromatteo ,&nbsp;Miriam Maiellaro,&nbsp;Lorenzo Sciuto,&nbsp;Grazia Bottillo,&nbsp;Emanuela Camera","doi":"10.1016/j.jcoa.2025.100265","DOIUrl":"10.1016/j.jcoa.2025.100265","url":null,"abstract":"<div><div>Free fatty acids (FFAs) are essential components of skin surface lipids (SSLs), which consist of a blend of epidermal and sebaceous lipids. The sebum component of SSLs is abundant in seborrheic body areas, which are rich in sebaceous glands (SGs). Sebum FFAs exhibit unique characteristics, including a prevalence of C14-C18 chain lengths, terminal branching, and a double bond at the Δ6 position. Notably, over one-third of the sebaceous FAs contain a single double bond. Deregulated synthesis of monounsaturated FAs (MUFAs) can lead to changes in sebum composition, which contribute to the pathogenesis of inflammatory skin conditions such as acne vulgaris, rosacea, psoriasis, and seborrheic dermatitis. A comprehensive characterization of the different isomers of unbound MUFAs distinguished by the position of the carbon-carbon double bond, has not been achieved in human sebum. Therefore, we aimed to develop an analytical strategy to differentiate the various carbon-carbon double bond positions in FFAs. Our methodology combines the Paternò-Büchi reaction, utilizing 2-acpy, with liquid chromatography and tandem mass spectrometry (LC-MS/MS). This strategy was initially optimized on standard FFAs and subsequently applied to human sebum. The method enabled the characterization of seventeen MUFAs with C14-C18 chain lengths and two C18 polyunsaturated FAs, namely linoleic and sebaleic acid. The prevalence of sapienic acid (C16:1n-10) among MUFAs supports the dominance of the Δ6 desaturation pathway catalyzed by the FADS2 enzyme in human SG. Additionally, the assay proved comparable abundance of MUFAs and PUFAs in sebum from males and females.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100265"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145219050","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":"Cutaneous volatile and semi-volatile organic compounds as markers of malaria-infection by wearable samplers and two-dimensional gas chromatography—time-of-flight-mass spectrometry","authors":"Daniel T. Pretorius ,&nbsp;Egmont R. Rohwer ,&nbsp;Yvette Naudé","doi":"10.1016/j.jcoa.2025.100233","DOIUrl":"10.1016/j.jcoa.2025.100233","url":null,"abstract":"<div><div>Malaria has been found to alter normal cutaneous volatile organic compound (VOC) profiles, suggesting their potential application as markers of <em>Plasmodium</em> infection. The cutaneous VOCs and semi-VOCs (SVOCs) of malaria-negative and -positive individuals, who visited two local clinics in the Vhembe district of Limpopo Province, South Africa, were extracted into wearable silicone rubber (polydimethyl siloxane [PDMS]) sampling bands adhered to the surface of the epidermis. After sampling of epidermal VOCs from participants the samplers were analysed by thermal desorption-comprehensive two-dimensional gas chromatography-time-of-flight-mass spectrometry (TD-GC × GC-TOFMS). Individual cutaneous VOCs and SVOCs profiles were constructed from these complex chromatographic profiles in order to identify potential signatures of <em>Plasmodium</em> infection. Fatty acid compounds associated with rancid malodour, and previously reported as mosquito attractants, were found at an overall greater abundance in chemical profiles of malaria-positive cases. A targeted analysis was performed for compounds previously reported to be associated with <em>Plasmodium</em> infection, viz., heptanal, (E)-2-octenal, 2-octanone, octanal, nonanal and (E)-2-decenal. The linearity (R²) range was 0.93–0.99 for a matrix matched (simulated cutaneous sampling) calibration range of 2.5–60 ng. Limits of detection (LOD) ranged from 0.4 pg (2-octanone) to 6.3 pg ((E)-2-octenal), whilst limits of quantification (LOQ) ranged from 1.4 pg to 21.1 pg. The mean percentage recoveries (<em>n</em> = 2) ranged from 77.8 % ((E)-2-decenal) to 118.9 % (2-octanone). The percentage relative standard deviations ( %RSDs; <em>n</em> = 2) ranged from &lt; 1 % for 2-octanone, octanal and nonanal to 27.1 % for (E)-2-octenal. We found that this particular suite of compounds, previously reported as indicators of malaria, was in fact non-specific for <em>Plasmodium</em> infection when compared to control subjects with comorbidities. A previously unreported (in a malaria-infection context) compound, (E)-2-octen-1-ol, correlated with malaria-positive participants, but was also observed for two malaria-negative participants, which could indicate latent malaria. In chronic cases, <em>Plasmodium vivax</em> can occur in reservoirs outside of the bloodstream, and thus blood-based diagnostic tests can miss latent infection. A key advantage of the epidermal sampler over blood tests is that the former collects whole-body organic compounds, and is therefore not limited to blood-borne markers of infection. As such it appears to be feasible for future investigations.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100233"},"PeriodicalIF":0.0,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144306606","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":"Chromatographic techniques in volcanic surveillance: from gases to dissolved species","authors":"María Asensio-Ramos","doi":"10.1016/j.jcoa.2025.100270","DOIUrl":"10.1016/j.jcoa.2025.100270","url":null,"abstract":"<div><div>Volcanic systems release chemical species in gases, aerosols, and hydrothermal or surface waters, providing critical insights into magmatic degassing, hydrothermal processes, and surface interactions that inform hazard assessment. Among the many chromatographic techniques available, volcanic surveillance has primarily relied on a few approaches. Gas chromatography (GC) and liquid chromatography (LC) are essential for analyzing these emissions, ranging from detecting permanent gases and volatile organic compounds (VOCs) in volcanic plumes to quantifying anions, cations, and organic compounds in dissolved phases such as hydrothermal waters and ash leachates. Advances in miniaturized GC instrumentation and hyphenated methods such as GC-mass spectrometry (MS) and LC-MS enhance the analysis of trace species, providing detailed insights into volcanic activity. Despite challenges posed by matrix complexity and the reactivity of some species, chromatography remains a key tool for investigating volcanic emissions and the processes driving them. This review highlights chromatographic methods applied to volcanic surveillance and the study of volcanic processes.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100270"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145264957","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":"Research advances in sample pretreatment techniques for pesticide residues","authors":"Jiarong Cui ,&nbsp;Fengshou Dong","doi":"10.1016/j.jcoa.2025.100259","DOIUrl":"10.1016/j.jcoa.2025.100259","url":null,"abstract":"<div><div>Pesticide residue analysis is fundamental to food safety and environmental protection, where sample pretreatment critically determines detection accuracy. This review examines the evolution from traditional methods (Soxhlet extraction, liquid-liquid extraction) to contemporary mainstream technologies (solid-phase extraction, QuEChERS, microextraction), and explores future prospects. Modern techniques like microextraction (SPME, DLLME) and magnetic solid-phase extraction (MSPE) have significantly enhanced efficiency while reducing solvent consumption by 90–95 %. The QuEChERS methodology has become the gold standard for multiresidue analysis in complex matrices. Future advancements focus on the miniaturization of analytical systems, suitable greener methodologies, and the development of advanced techniques for complex matrices and ultra-trace analysis.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100259"},"PeriodicalIF":3.2,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145158056","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}