Journal of Chromatography A最新文献

{"title":"Optimizing retention time and peak width reproducibility with high peak capacity in high-speed gas chromatography using dynamic pressure gradient injection","authors":"Austin D. Dobrecevich ,&nbsp;Joel A. Thornton ,&nbsp;Robert E. Synovec","doi":"10.1016/j.chroma.2025.465889","DOIUrl":"10.1016/j.chroma.2025.465889","url":null,"abstract":"<div><div>We are developing high speed gas chromatographic (HSGC) instrumentation with an optimizable injection system, referred to herein as dynamic pressure gradient injection (DPGI). In the present study, we examine the effects of the DPGI pulse width and linear flow velocity on the resultant chromatographic peak widths and separation peak capacity. DPGI readily yields reproducible peak widths and retention times in a sub-second separation runtime regime over long periods of repeated injections. These repeated measurements facilitate a statistically rigorous analysis of the relationships between peak widths obtained and injection pulse width and/or linear flow velocity. Chromatographic performance was studied using a 1 <em>m</em> × 100 µm × 0.1 µm Rtx-5 chromatographic column at various linear flow velocities with hydrogen as the carrier gas, an isothermal temperature of 100 °C, with a test mixture of acetone, nonane, decane and undecane. At this column temperature, acetone is nominally unretained. For conditions where plate height is minimized (<em>H</em>_min) at the so-called optimum linear flow velocity, <em>u</em>_opt, and with the off-column band broadening approaching zero by optimizing DPGI performance, an <em>H</em>_min of 77 µm was obtained. The chromatographic data corresponding to this <em>H</em>_min included a minimum peak width-at-half height (<span><math><mrow><msub><mi>w</mi><mrow><mn>1</mn><mo>/</mo><mn>2</mn></mrow></msub><mrow><mo>)</mo></mrow></mrow></math></span> of <span><math><mrow><mn>8</mn><mo>±</mo><mn>0.2</mn><mspace></mspace><mi>m</mi><mi>s</mi></mrow></math></span> for acetone, and a peak capacity (<span><math><mrow><msub><mi>n</mi><mi>c</mi></msub><mrow><mo>)</mo><mspace></mspace></mrow></mrow></math></span>of ∼30 for a separation runtime of 1.2 s. When all that is needed is the separation of a few key analytes as fast as possible, and if some peak capacity can be sacrificed, the fastest separation studied yielded a minimum peak width at half-height <span><math><mrow><msub><mi>w</mi><mrow><mn>1</mn><mo>/</mo><mn>2</mn></mrow></msub><mo>=</mo><mn>5.5</mn><mspace></mspace><mo>±</mo><mn>0.09</mn><mspace></mspace><mi>m</mi><mi>s</mi></mrow></math></span> for acetone, and a <span><math><msub><mi>n</mi><mi>c</mi></msub></math></span> of 10 with a separation runtime of <span><math><mrow><mn>325</mn><mspace></mspace><mi>m</mi><mi>s</mi><mo>.</mo></mrow></math></span></div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465889"},"PeriodicalIF":3.8,"publicationDate":"2025-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143704438","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Fast unmasking toxicity of safe personal care products","authors":"Gertrud E. Morlock ,&nbsp;Luisa Zoller","doi":"10.1016/j.chroma.2025.465886","DOIUrl":"10.1016/j.chroma.2025.465886","url":null,"abstract":"<div><div>Personal care products are used several times a day and come into contact with the skin for many hours. As hazard-related data on products are rare, an imaging safety screening was developed. For the first time, it detected known and unknown hazardous compounds in 140 personal care products from 20 different product segments, including beauty and lifestyle products. The evidence-based chromatographic–hazard-related profiling detected genotoxic, cytotoxic, and estrogenic compounds, which were assigned to structural groups, and revealed that personal care products are not as safe as stated. Wound-healing and nipple creams in contact with babies as well as lipsticks used by adolescents were shown to contain highly toxic compounds able to enter the bloodstream via wounds, micro-injuries or bleeding gums and contaminate nature when washed off. Dose-response curves pointed to half-maximal genotoxic effect doses (EC₅₀) of around 60 µg of such products which can easily be exceeded by a factor of 100,000 for only 6 g product applied or for an aggregated use of various products increasing genotoxic exposure, as observed in consumer profiles. Simulated metabolization via S9 liver enzymes did not lead to detoxification. The new safety screening not only unmasked quickly the toxicity of personal care products but also provided an understanding of how to produce hazard-free products. It empowers industries to produce future products in compliance with their standards and claims in terms of consumer health, ethics, environmental compatibility, and sustainability, and authorities to control the safety of products on the market and tackle the current underregulation.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465886"},"PeriodicalIF":3.8,"publicationDate":"2025-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143844132","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A 3D-metal-printed UV detector specifically designed for real-time monitoring of an open column chromatography fraction","authors":"Yanting Liu ,&nbsp;Xiaochun Li ,&nbsp;Hongjun Luo ,&nbsp;Rui Huang ,&nbsp;Xuewan Wu ,&nbsp;Lei Tan ,&nbsp;Jialiang Guo ,&nbsp;Kaisong Yuan","doi":"10.1016/j.chroma.2025.465884","DOIUrl":"10.1016/j.chroma.2025.465884","url":null,"abstract":"<div><div>We developed a three-dimensional (3D)-metal-printed ultraviolet (UV) detector with an aluminum alloy housing that allows it to withstand low-polarity organic solvents. The detector can be attached to the lower end of an open chromatography column to realize real-time monitoring of the separated and eluted colorless fractions. Open column chromatography is commonly used for the separation and purification of mixtures. However, the direct combination of open chromatography column with 3D-metal-printed UV detectors is rarely reported. In the context of open column chromatography experiments, thin-layer chromatography (TLC) is typically employed for the qualitative analysis of separated products. Nevertheless, this approach is both cumbersome and time-consuming. Therefore, to reduce workload and save time, we developed a 3D-metal-printed UV detector, which exhibits good stability and linearity (R²&gt; 0.99). The feasibility of real-time monitoring using this 3D-metal-printed UV detector was verified by subjecting the mixture to separation and monitoring. On elution of a substance exhibiting light-absorbing properties, a decrease in voltage is observed. At this point, the collection of the fractions may be initiated to achieve the effect of substance tracking. The utilization of the 3D-metal-printed UV detector for real-time monitoring enables the elimination of the time previously spent on the collection of all fractions and the subsequent determination of whether the fractions contain the substance by TLC. It is also capable of determining the separation effect of the mixture based on the curve monitored in real time. Moreover, the device can modify the dimensions of the interface, thereby facilitating its utilization in conjunction with high-performance liquid chromatography (HPLC) for the real-time monitoring of the separation effect of the column. The device is characterized by low cost and small size.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465884"},"PeriodicalIF":3.8,"publicationDate":"2025-03-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143715979","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Hydrolysis reaction paths and kinetics of cationic bleaching activators with different leaving groups based on LC-MS and HPLC","authors":"Fuyang Gu ,&nbsp;Xiaoyan Wang ,&nbsp;Jinmei Du ,&nbsp;Yang Jiang ,&nbsp;Dagang Miao ,&nbsp;Yanmei Qu ,&nbsp;Dongyan Shao ,&nbsp;Guowei Xiao ,&nbsp;Changhai Xu","doi":"10.1016/j.chroma.2025.465883","DOIUrl":"10.1016/j.chroma.2025.465883","url":null,"abstract":"<div><div>Cationic bleaching activators can effectively achieve low-temperature bleaching in hydrogen peroxide system, but at the same time, self-hydrolysis reaction will occur to affect the low-temperature bleaching effect, and the complex hydrolysis pathways of cationic bleaching activators are still elusive. In this paper, the hydrolysis reaction pathways, mechanisms, rates and kinetics of cationic bleaching activators N-[4-(triethylaminomethyl)benzoyl]lactam chlorides (TBLCs) with different lactam leaving groups were investigated in depth by liquid chromatography-mass spectrometry (LC-MS) and high-performance liquid chromatography (HPLC). Specifically, we characterized the hydrolysis products by LC-MS and further quantified the hydrolysis products using HPLC, demonstrating that the hydrolysis can take place via two pathways, generating chain-breaking products and ring-opening products, and that both react at different rates depending on the different lactam leaving groups. Notably, the quantitative results showed that the chain-breaking products were always larger than the ring-opening products, and the chain-breaking products were ineffective for bleaching, which was the main reason for the decrease in the bleaching performance of TBLCs. The mechanism of hydrolysis is discussed and the reaction rate was determined to follow first-order kinetics using HPLC. We have successfully delineated the complete transformation pathway of the hydrolysis reaction using this method, providing valuable information for the future preparation of novel bleaching activators and the reduction of this reaction.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465883"},"PeriodicalIF":3.8,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143685434","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Current experimental, statistical, and mechanistic approaches to optimizing biomolecule separations in aqueous two-phase systems","authors":"Seth A Kriz,&nbsp;Caryn L Heldt","doi":"10.1016/j.chroma.2025.465881","DOIUrl":"10.1016/j.chroma.2025.465881","url":null,"abstract":"<div><div>Aqueous two-phase systems (ATPS) have been used to purify a range of biomolecules, including small molecules, monoclonal antibodies, viruses, and whole cells. They are known for selective separations, creating a stabilizing, low-shear environment, and high yields. Recently, as biomanufacturing attempts to adopt continuous processing, attention has shifted to ATPS for its ability to operate fully continuously while incurring lower costs than many chromatographic methods. But despite 60 years of exploration and development, the complex network of interlinked driving forces controlling these separations has prevented robust development of process understanding, and most ATPS separations are still optimized using slow and costly manual screening methods. As a result, industry has been unwilling to adopt ATPS. Fortunately, a growing body of literature is developing statistical and mechanistic models of ATPS to predict liquid-liquid equilibria and separations with reduced experimental burden. This review surveys the application of these models to ATPS, comparing their progress and potential to promote rapid development of bioseparations in the near and long term. The discussion evaluates the adaptability of statistical tools, like response surface methodology and artificial neural networks, and contrasts it with the process understanding generated through application of semi-empirical thermodynamic models. Strategies are explored to automate optimization of separations for new biomolecules using these models to create artificial data. By understanding the landscape of models applied to ATPS, this review will start a discussion about bringing this technology closer to commercialization and enabling continuous processing on a broader scale.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465881"},"PeriodicalIF":3.8,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143685507","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Use of a centrifuge in solid-phase extraction is a valid platform for cleanup in the high-throughput analysis of chemical contaminants in nonfatty and fatty foods","authors":"Nicolás Michlig ,&nbsp;Steven J. Lehotay","doi":"10.1016/j.chroma.2025.465882","DOIUrl":"10.1016/j.chroma.2025.465882","url":null,"abstract":"<div><div>In recent years, the “quick, easy, cheap, effective, rugged, safe, efficient, and robust” (QuEChERSER) mega-method was developed for sample preparation and analysis of pesticides, environmental contaminants, veterinary drugs, and other residues in a wide variety of foods. In addition to wider analytical scope, QuEChERSER has many other advantages over the previous QuEChERS method, such as better cleanup for improved quality of results. For example, automated robotic mini-cartridge solid-phase extraction (µ-SPE) has been shown to provide excellent cleanup prior to gas chromatography - tandem mass spectrometry (GC-MS/MS) analysis. However, not all laboratories have the resources and expertise needed to adopt the robotic method. To address this limitation, a new approach is herein introduced using centrifugal µ-SPE as a simpler and lower-cost alternative using the same commercial mini-cartridges as the robotic version. In this study, both robotic and centrifugal µ-SPE were compared for the cleanup of QuEChERS and QuEChERSER extracts of 10 commodities (avocado, blueberry, egg, mixed grains, honey, bovine kidney/liver, whole milk, black olive, spinach, and tilapia) in the low-pressure GC-MS/MS analysis of 245 pesticides and environmental contaminants. QuEChERS extracts overwhelmed the sorbents in the mini-cartridges in most cases, leading to less cleanup and worse performance in the most complex matrices, but the 4-fold more dilute QuEChERSER extracts avoided that problem while still meeting detection limit needs. This study demonstrated that graphitized carbon black (GCB) was not needed for cleanup of samples that did not contain chlorophyll, and inclusion of more than 1 mg of GCB in the mini-cartridges led to &lt;3 % recovery of certain structurally planar analytes. In QuEChERSER, analyte recoveries averaged 99 % in all matrices using both robotic and centrifugal µ-SPE, but robotic liquid handling demonstrated better precision of 4 % RSD compared to 6 % using the centrifugal option. Cleanup was also slightly better using robotic automation. Laboratories may choose either option in QuEChERSER (or QuEChERS) to achieve better cleanup, analytical performance, and greater ruggedness than the dispersive-SPE format commonly employed in this application for the past 20 years.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465882"},"PeriodicalIF":3.8,"publicationDate":"2025-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143673047","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"High-resolution mass spectrometry-based assessment of chemical composition's effect on the honey color","authors":"Zhiwei Sun ,&nbsp;Lanhua Liu ,&nbsp;Hui Zhang ,&nbsp;Mingzhu Zhang ,&nbsp;Boyang Xu ,&nbsp;Yousheng Wang ,&nbsp;Xingjiang Li ,&nbsp;Dongdong Mu ,&nbsp;Xuefeng Wu","doi":"10.1016/j.chroma.2025.465880","DOIUrl":"10.1016/j.chroma.2025.465880","url":null,"abstract":"<div><div>Honey is a nutrient-rich natural functional food, with its color being considered as a key indicator of quality and consumer acceptance. Although various secondary metabolites are closely related to the color of honey, the specific substances and their exact effects on honey color remain unclear. In this study, the chemical composition, such as organic acids, polyphenols and vitamins, in different colored honey (<em>Acacia, buckwheat, linden, vitex, lychee</em> and <em>jujube</em> honey) were quantitatively analyzed using liquid chromatography-high resolution mass spectrometry (LC<img>HRMS). The correlations between the chemical composition and the honey color were established by the mantel test. The results showed that quinic acid, ascorbic acid, and other composition were identified as significantly related with honey color. The validation experiments indicated that adding these significantly related substances to honey samples could multiplicatively deepen the honey color, and the value of the deepening color was positively correlated with that of the initial color. The study developed a practical and systematic LC<img>HRMS method for analyzing chemical composition in honey. The results provided valuable scientific insights into the relationship between chemical composition and honey color. Additionally, it introduced a novel and feasible approach for investigating the effects of substances on the color of complex mixture systems.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1748 ","pages":"Article 465880"},"PeriodicalIF":3.8,"publicationDate":"2025-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143654565","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Identification of aldose reductase inhibitors from the flowers of Tussilago farfara using PCN-222 metal-organic framework-based immobilization-free affinity selection coupled with high-performance liquid chromatography","authors":"Zhaoyang Wu ,&nbsp;Jiayin Tian ,&nbsp;Xuelian Xin ,&nbsp;Jinlu Tian ,&nbsp;Soon Sung Lim ,&nbsp;Hongyuan Yan ,&nbsp;Zhiqiang Wang","doi":"10.1016/j.chroma.2025.465879","DOIUrl":"10.1016/j.chroma.2025.465879","url":null,"abstract":"<div><div>Inhibition of aldose reductase (AR) activity is promising for mitigating diabetic complications. This study proposed a novel screening approach combining PCN-222 metal-organic framework (MOF)-based immobilization-free affinity selection with high-performance liquid chromatography to identify AR inhibitors (ARIs) from natural product extracts. As a proof-of-concept, the AR inhibitory activity of the flowers of <em>Tussilago farfara</em> L. (FTF) was evaluated, and ARIs in FTF were identified using the proposed approach. To validate the screening results, major constituents of FTF were isolated for functional assays, inhibitory kinetics, and interaction mechanisms. The results demonstrated significant inhibitory activity of FTF extracts against AR (IC₅₀ = 3.49 µg/mL), with chlorogenic acid (IC₅₀ = 0.97 µM, <em>K</em>_i = 1.21 µM, <em>K</em>_a = 4.88 × 10⁴ L/mol), isochlorogenic acid A (IC₅₀ = 0.76 µM, <em>K</em>_i = 0.61 µM, <em>K</em>_a = 5.25 × 10⁴ L/mol), isochlorogenic acid C (IC₅₀ = 1.83 µM, <em>K</em>_i = 1.24 µM, <em>K</em>_a = 4.25 × 10⁵ L/mol), and isochlorogenic acid B (IC₅₀ = 0.95 µM, <em>K</em>_i = 0.40 µM, <em>K</em>_a = 3.64 × 10⁴ L/mol) identified using the proposed method, where all exhibited high binding affinity to AR. In contrast, rutin (IC₅₀ = 3.69 µM, <em>K</em>_i = 5.60 µM, <em>K</em>_a = 2.93 × 10⁴ L/mol), despite being confirmed as an ARI, exhibited weaker binding affinity to AR and was not identified by this approach. These findings demonstrate the effectiveness of the proposed method for efficiently identifying enzyme inhibitors with high binding affinities, and represent the first application of MOFs in immobilization-free affinity selection screening methods.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1748 ","pages":"Article 465879"},"PeriodicalIF":3.8,"publicationDate":"2025-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143672880","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Advancing profiling of secondary antioxidant metabolites in Allium cepa PDO leaf extract: Online comprehensive two-dimensional liquid chromatography with high-resolution mass spectrometry and pre-column DPPH assay","authors":"Giovanna Aquino ,&nbsp;Eduardo Maria Sommella ,&nbsp;Emanuela Salviati ,&nbsp;Michele Manfra ,&nbsp;Giulia Auriemma ,&nbsp;Pietro Campiglia ,&nbsp;Giacomo Pepe ,&nbsp;Manuela Giovanna Basilicata","doi":"10.1016/j.chroma.2025.465877","DOIUrl":"10.1016/j.chroma.2025.465877","url":null,"abstract":"<div><div>The food and agricultural processing industries generate significant amounts of phenolic-rich by-products, which hold potential as natural antioxidant sources for a wide range of applications, including functional ingredients and nutraceutical formulations. <em>Allium cepa</em> leaves represent a promising source of bioactive compounds. However, due to the complexity of their chemical composition, advanced analytical techniques are required to fully characterize the secondary metabolite profile and identify specific phytochemical classes or fractions with high nutraceutical potential. In this context, an online comprehensive two-dimensional liquid chromatography (LC×LC) approach was developed and optimized for the in-depth characterization of the phytochemical profile of <em>Allium cepa</em> PDO leaf extract. Key parameters in both dimensions, including flow rate, stationary phase chemistry, and mobile phase composition, were investigated to enhance peak capacity and orthogonality. The optimized method combined reversed phase in both dimension (RP-LC×RP-LC), offering high orthogonality (<em>A₀</em>: 70.46 %) and peak capacity (<em>n_c</em>: 1788.88). and significantly improving the separation of multiple secondary metabolite classes by effective employment of the 2D separation space. Further hyphenation with high-resolution mass spectrometry (HRMS), enhanced compound annotation compared to mono-dimensional (1D-LC) techniques. A total of 147 compounds were tentatively annotated belonging to multiple classes such as flavonoids, saponins, phenylpropanoids, isoprenoids, terpenes, dipeptides, fatty acids, and lipids. Additionally, the antioxidant activity of <em>Allium cepa</em> leaf extract was assessed by coupling a pre-column 2,2-diphenyl-1-picrylhydrazyl (DPPH) assay with the LC×LC-DAD-HRMS platform. This integrated approach enabled the identification of individual contributions of flavonoids, isoprenoids, and phenylpropanoids to radical scavenging activity.</div><div>The method allowed an in-depth exploration of <em>Allium cepa</em> phytochemical profile, demonstrating to hold significant potential for the standardization of antioxidant biomarkers, with promising applications in the nutraceutical industry.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465877"},"PeriodicalIF":3.8,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143685436","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Combining per-aqueous and chiral reversed phase separation modes towards an enhanced comprehensive 2-dimensional liquid chromatographic based chiral screening platform","authors":"Turaj Rahmani ,&nbsp;Elena Bandini ,&nbsp;Stephanie A. Schuster ,&nbsp;Lander Iterbeke ,&nbsp;Jean-François Focant ,&nbsp;Frédéric Lynen","doi":"10.1016/j.chroma.2025.465875","DOIUrl":"10.1016/j.chroma.2025.465875","url":null,"abstract":"<div><div>The differentiation of enantiomers in complex mixtures is crucial in various fields such as food science, pharmaceuticals, and environmental studies. While this is achievable in principle through comprehensive two-dimensional liquid chromatography (LC × LC), practical challenges emerge when the mobile phase used in the first dimension (¹D) is too strong or incompatible with the one in the second dimension (²D), leading to peak broadening and reduced resolution. These drawbacks become particularly evident when analyzing a diverse range of chiral compounds. In order to obtain timely elution of such compounds, typically spanning a range of hydrophobicity, the use of gradients (in both dimensions) is inevitable. This in turn leads to changing mobile phase compositions transferred from ¹D to ²D, and hence to variations in the effectiveness of the modulation process. Lowering of the eluotropic strength of the mobile phase used in ¹D allows to mitigate such problems. In this study, a novel achiral × chiral platform for fully automated screening of chiral compounds was developed. In the ¹D of this platform, reversed HILIC (or per-aqueous liquid chromatography (PALC)) was employed, utilizing a commercially available HILIC column, which ensures robust and reproducible results with a water-rich mobile phase. In ²D, chiral chromatography with a broad range of gradients was utilized. Moreover, the impact of varying concentrations of organic solvent transferred to the ²D on enantioseparation was investigated. The water-rich mobile phase in the ¹D facilitates the complete refocusing of organic solutes before entering the second dimension, preventing the loss of resolution in the ²D. This also allows for longer sampling times, consequently longer ²D running times, reducing the need for ultra-fast columns in the ²D. Furthermore, it enables the application of various mobile phase compositions in the ²D. Finally, this tool was successfully used to analyze compounds in urine and plasma matrices.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1748 ","pages":"Article 465875"},"PeriodicalIF":3.8,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143654563","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}