Journal of separation science最新文献

{"title":"Separation and Quantification of Cyclic di-AMP, -GMP, and Cyclic GAMP in Bacteria Using LC–MS/MS","authors":"Silvio Uhlig,&nbsp;Kristina Vevik,&nbsp;Joke Van De Vyver,&nbsp;Inger Sofie Dragland,&nbsp;Lene A. Grutle,&nbsp;Maria Pain,&nbsp;Roger Simm","doi":"10.1002/jssc.70157","DOIUrl":"https://doi.org/10.1002/jssc.70157","url":null,"abstract":"<div>\u0000 \u0000 <p>This study summarizes the optimization of a selective method for UHPLC-separation and subsequent tandem mass spectrometric detection of adenosyl- and guanosyl-containing cyclic dinucleotides in bacteria. Cyclic dinucleotides are a class of bacterial second messenger molecules, and their cellular concentrations are tightly regulated by biosynthesis and enzymatic breakdown. Although bacteria, according to present knowledge, only produce 3′,3′-linked cyclic dinucleotides, other nucleotide variants also exist, including structural isomers, which may lead to misidentifications. Mixtures of the 2′,2′-, 2′,3′-, and 3′,3′-linked isomers of cyclic di-AMP, cyclic di-GMP, and cyclic GAMP were separated using an octadecylsilane-amide column. Subsequent tandem mass spectrometric detection was based on monitoring the adenosyl- or guanosyl-product ions for quantification, and additional monitoring of up to three product ions for verification. We show the presence of an unidentified putative structural isomer of cyclic di-AMP in several bacterial species. Cyclic di-AMP was quantified using an isotope dilution approach and ¹⁵N₁₀-cyclic di-AMP as an internal standard, whereas instrument calibration for other variants was performed using matrix-matched calibration. The combined measurement uncertainty u′ for the quantification of the nine cyclic dinucleotide variants in anion-exchanged bacterial extracts was 10%–41%, determined at an extract concentration of 12 nM. Our study also demonstrated the application of total protein measurements in resuspended, nucleotide-extracted, bacterial pellets to normalize nucleotide concentrations.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143901081","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analysis of Phthalate Monoesters and Bisphenols in Human Prostate Cancer Tissue and Urine","authors":"Tianai Zhang,&nbsp;Jiaqi Guo,&nbsp;Weiyang Sun,&nbsp;Xinyi Huang,&nbsp;Zilong Zhang,&nbsp;Yuming Jin,&nbsp;Zifan Hu,&nbsp;Shi Qiu,&nbsp;Xiaoli Zou","doi":"10.1002/jssc.70154","DOIUrl":"https://doi.org/10.1002/jssc.70154","url":null,"abstract":"<div>\u0000 \u0000 <p>A growing concern has been raised about human exposure to phthalates and bisphenols, while data is limited regarding the accumulation of these endocrine disrupting chemicals at the target tissue. In this study, a novel, simple, and sensitive method was successfully developed for the simultaneous determination of nine phthalate monoesters and nine bisphenols in human prostate tissue samples. A solid–liquid extraction procedure was applied following ultra-high performance liquid chromatography tandem mass spectrometry analysis. The detection and quantification limits were in the range of 4.12 × 10⁻³ to 0.370 ng/g and 1.38 × 10⁻³ to 1.23 ng/g, respectively. The average spiked recoveries varied from 71.4% to 102%, with relative standard deviations ≤ 10%. Finally, this method was applied to 76 human prostate tissue samples. Four phthalate monoesters (mono-ethyl phthalate, mono-<i>iso</i>-butyl phthalate, mono-<i>n</i>-butyl phthalate, and mono-benzyl phthalate) were detected with the highest frequency of 98.68%, followed by other five phthalate monoesters (71.05% ∼ 94.74%), bisphenol S (72.37%), and bisphenol A (57.89%). Five bisphenols were not detected in any tissue sample. The concentrations of detected phthalate monoesters and bisphenols ranged from 1.12 × 10⁻³to 1.86 × 10² ng/g and 6.08 × 10⁻³to 39.0 ng/g, respectively, with standard errors ranging from 3.25×10⁻³to 4.64 ng/g. Besides, a positive correlation for the concentration of seven phthalate monoesters and bisphenol A could be observed between tissue and urine, which indicates that these metabolites in urine can serve as noninvasive biomarkers to evaluate the true exposure level of prostate tissue. This study provides data and information on exposure to phthalate monoesters and bisphenols in human prostate tissue and the association with their urinary metabolites, supporting further studies of pollutant exposure and prostate disease.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143879879","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Extended Steroid Profiling in Human Serum and Plasma With Simultaneous Quantitative Determination Using One-Point Internal Calibration","authors":"Mathieu Galmiche,&nbsp;Oriane Strassel,&nbsp;Marie-Anaïs Monat,&nbsp;Isabel Meister,&nbsp;Julien Boccard,&nbsp;Serge Rudaz","doi":"10.1002/jssc.70147","DOIUrl":"https://doi.org/10.1002/jssc.70147","url":null,"abstract":"<div>\u0000 \u0000 <p>Steroids are a major set of endogenous bioactive compounds. Although increasingly popular, their analysis in biofluids by LC-MS is associated with enduring challenges, such as their low endogenous concentrations or the coexistence of numerous isobaric compounds. Their natural presence in biological matrices complicates their absolute quantification in blood, as the obtention of a blank matrix to establish an external calibration curve is impossible. This protocol describes a strategy for developing an LC-MS/MS method for the extended profiling of steroids in serum and plasma, including as much as 171 target compounds, with the additional absolute quantification of four main steroids (cortisol, testosterone, progesterone, and androstenedione). The proposed sample preparation involves protein precipitation in organic solvents and subsequent filtration of the sample on HLB cartridge. The LC method is developed to resolve most isobaric species thanks to a biphenyl stationary phase. MS detection is performed in multiple reaction monitoring mode with post-column addition of ammonium fluoride to enhance sensitivity. A one-point internal calibration strategy is presented for the absolute quantification of endogenous steroids. The application of this method to the NIST Plasma Reference Material (SRM 1950) led to the identification of 69 distinct endogenous steroids, making it the most comprehensive profiling of these compounds in this reference matrix to date. The quantitative performance of the method is assessed with two certified materials and shows satisfactory precision and trueness.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861672","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simultaneous Determination of Multiple Anti-Seizure Medications in Human Plasma Using High-Performance Liquid Chromatography-Tandem Mass Spectrometry with Positive/Negative Ion-Switching Ionization Mode for Therapeutic Drug Monitoring","authors":"Yu-Fei Zhang,&nbsp;Zheng Yu,&nbsp;Zhao Zhao,&nbsp;Le-Qing Xu,&nbsp;Xun-Yi Wu,&nbsp;Chun-Lai Ma","doi":"10.1002/jssc.70151","DOIUrl":"https://doi.org/10.1002/jssc.70151","url":null,"abstract":"<div>\u0000 \u0000 <p>Monotherapy or combination therapy with anti-seizure medications (ASMs) remains the cornerstone of epilepsy treatment. Therapeutic drug monitoring is important for individualized ASM treatment and for optimizing outcomes in patients with epilepsy. Therefore, the simultaneous and accurate quantification of ASMs is necessary and helpful for clinical use. In this study, a new method was developed to simultaneously quantify carbamazepine, lacosamide, lamotrigine, levetiracetam, oxcarbazepine, perampanel, sodium valproate, topiramate, and an active metabolite of oxcarbazepine, 10, 11-dihydro-10-hydroxycarbamazepine, in human plasma by high-performance liquid chromatography-tandem mass spectrometry using the positive/negative ion-switching ionization mode. The method was assessed for accuracy, precision, linearity, recovery, and matrix effects according to the criteria of the U.S. Food and Drug Administration Bioanalytical Method Validation Guidelines for Industry for Bioanalytical Methods. The lower limit of quantification was determined to be 0.001–25 µg/mL for each analyte. The intra- and inter-day precision values had &lt;14.6% coefficients of variation, and the accuracy ranged from 85.3% to 113% at the three levels of quality control. In addition, this method was successfully applied to therapeutic drug monitoring of ASMs in patients with epilepsy. This method allows for simple preparation, accurate quantification, and the determination of different ASMs without requiring analytical method switching, making it particularly suitable for therapeutic drug monitoring in busy clinical and hospital laboratory settings.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861454","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Nickel–Cobalt-Layered Double Hydroxide and Carbon Composite for Monitoring the Plasticizers Migrated Into Hot Tea Drinks","authors":"Mir Ali Farajzadeh,&nbsp;Zahra Asghari,&nbsp;Sakha Pezhhanfar,&nbsp;Mohammad Reza Afshar Mogaddadam","doi":"10.1002/jssc.70146","DOIUrl":"https://doi.org/10.1002/jssc.70146","url":null,"abstract":"<div>\u0000 \u0000 <p>In this study, a metal–organic framework-derived layered double hydroxide named nickel–cobalt-layered double hydroxide was synthesized from ZIF-67 and mixed with activated carbon to prepare a suitable sorbent for dispersive micro solid phase extraction. It was used to extract plasticizers from the tea infusions. To develop the method, the composite adsorbed the analytes through vortexing in a solution containing dissolved NaCl. Subsequently, to separate the sorbent particles, centrifugation was used. A desorption solvent composed of methanol and 3-picoline was utilized via vortexing to release the plasticizers from the sorbent. Subsequently, 1,2-dibromoethane at the µL level was eked into the desorption solvent, and the resulting mixture was injected into an aqueous solution containing dissolved NaCl. The obtained cloudy solution was subjected to centrifugation, and an aliquot of the settled extractant was injected into a gas chromatograph equipped with a flame ionization detector. Favorable extraction recoveries (ranging from 36% to 89%), high enrichment factors (180–445), low limits of detection (0.65–4.01 µg L⁻¹), good intra- (2.64%–3.82%) and inter-day (3.06%–6.95%) relative standard deviations, and wide linear ranges of the calibration curves were recorded. Applying an anti-solvent-oriented workup section to increase the yield of ZIF-67, production of the composite, and its application in sample preparation for the first time were novel aspects of the research.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861452","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Chinese Herbal Medicine Residue-Derived Biochar Assisted Matrix Solid Phase Dispersion Microextraction of Synthetic Dyes From Lake Sediments Using Supramolecular Solvents as Dispersing Solvents","authors":"Zhehui Weng,&nbsp;Yang Yu,&nbsp;Wenxu Hu,&nbsp;Ru Yang,&nbsp;Yao Huang,&nbsp;Dandan Ge","doi":"10.1002/jssc.70149","DOIUrl":"https://doi.org/10.1002/jssc.70149","url":null,"abstract":"<div>\u0000 \u0000 <p>In this study, a new matrix solid-phase dispersion (MSPD) method was developed and applied to extract auramine O (AO) and rhodamine B (RB) from sediment samples. A new supramolecular solvent (SUPRAS) composed of hexafluorobutanol (HFB) and linaool was used as the dispersing solvent of MSPD. Biochar, obtained by pyrolysis of a Chinese medicine residue namely <i>Sophora japonica</i> L., was used as the dispersing sorbent of MSPD procedure. Parameters influencing the extraction efficiency including the type and volume of dispersing solvent, amount of dispersing sorbent, grinding period, and vortex time were investigated and optimized. Under the optimized conditions, the linear range of the target analytes was 3–400 µg g⁻¹ with correlation coefficients higher than 0.9964. The method provided low limits of detection and limits of quantification, and excellent precision (intra- and inter-day analysis with relative standard deviations below 5.5%). Finally, the proposed method was applied to determine the synthetic dyes in Dianchi Lake sediments with satisfactory extraction recoveries of 93.5%–105.1%, indicating the applicability for the determination of synthetic analytes in real samples. Compared with the traditional sample preparation method for sediment samples, the proposed method reduced the extraction time, sample, and organic solvent usage. The proposed method is easy, fast, and green and can be applied to determine various analytes in sediment samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861453","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Are We Ready for It? A Review of Forensic Applications and Readiness for Comprehensive Two-Dimensional Gas Chromatography in Routine Forensic Analysis","authors":"Emma L. Macturk,&nbsp;Kevin Hayes,&nbsp;Gwen O'Sullivan,&nbsp;Katelynn A. Perrault Uptmor","doi":"10.1002/jssc.70138","DOIUrl":"https://doi.org/10.1002/jssc.70138","url":null,"abstract":"<p>Comprehensive two-dimensional gas chromatography (GC×GC) has been explored in forensic research to provide advanced chromatographic separation for forensic evidence, including illicit drugs, fingerprint residue, chemical, biological, nuclear, and radioactive (CBNR) substances, toxicological evidence, odor decomposition, and petroleum analysis for arson investigations and oil spill tracing. In GC×GC, the separation and analysis of analytes is similar to one-dimensional GC, but the primary column is connected to a secondary column via a modulator to provide two independent separation mechanisms, thus increasing the peak capacity of the analysis. The goal of implementing GC×GC in forensic studies is often to increase the separation and detectability of analytes and has most often been applied in nontargeted forensic applications where a wide range of analytes must be analyzed simultaneously. To date, there has been no summary of the current state of forensic research that evaluates both analytical and legal readiness for routine use. For these analytical methods to be adopted into forensic laboratories and be used in evidence analysis, they must meet rigorous analytical standards. In addition, new analytical methods for evidence analysis must adhere to standards laid out by the legal system, including the Frye Standard, Daubert Standard, and Federal Rule of Evidence 702 in the United States and the Mohan Criteria in Canada. Current research on GC×GC use for forensic applications was summarized and reviewed for analytical advances and technology readiness to provide a comprehensive view of GC×GC use for future routine implementation. A technology readiness scale, with levels from 1 to 4, was used to characterize the advancement of research in each individual application area. Seven forensic chemistry applications are discussed related to courtroom criteria and categorized into technology readiness levels based on current literature as of 2024. Future directions for all applications should place a focus on increased intra- and inter-laboratory validation, error rate analysis, and standardization.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70138","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143856858","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Measuring Nitrite and Nitrate in Rain and River Water Samples Using a Portable Ion Chromatograph in Step-gradient Mode and High Sensitivity Detection Flow Cell","authors":"Yonglin Mai,&nbsp;Kurt Debruille,&nbsp;Ibraam Mikhail,&nbsp;Vipul Gupta,&nbsp;Eoin Murray,&nbsp;Roman Frantsuzov,&nbsp;Brett Paull","doi":"10.1002/jssc.70134","DOIUrl":"https://doi.org/10.1002/jssc.70134","url":null,"abstract":"<p>With the increasing environmental pollution issues, there is a growing need for sensitive and real-time monitoring of pollutants. Nitrite and nitrate are common nutrients that are related to water quality. This study aims to enhance nitrate and nitrite detection capabilities using a portable ion chromatography-based nutrient analyzer, Aquamonitrix. By optimizing it for ultra-low detection limits (LODs), we address challenges in environmental water quality assessment in Tasmania, Australia. Using step-gradient mode with a stereolithography three-dimensional printed flow cell with a 5 cm optical path length, a 300 µL injection loop, and 60 mM KOH as eluent, LODs of 0.004 µg/mL for nitrite and 0.023 µg/mL for nitrate were achieved. Further improving to 0.008 µg/mL for nitrate with a 10 cm optical path length flow cell and 120 mM NaCl as eluent. A repeatability assessment over 84 automatic runs showed a relative standard deviation under 1.42% for peak area and 0.49% for retention time. The system demonstrated tolerance to salinity, handling up to 5 parts per thousand in artificial seawater. Comparative analysis of environmental samples revealed that nitrate levels in Tasmanian rainwater were five times lower than in Ireland. An average concentration of 2.08 µg/mL nitrate was found in Tamar River samples, aligning with local commercial lab data. Real-time, on-site analysis along the Derwent River detected an average nitrate concentration of 0.17 µg/mL. Validation against conventional standard ion chromatography showed no significant differences (<i>p</i> &gt; 0.05), underscoring Aquamonitrix's robustness for field-based water quality monitoring. A 5-day deployment of Aquamonitrix further demonstrated the system's reliability under significant temperature fluctuations between day and night.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70134","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143856994","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Affinity Capillary Electrophoresis Based on Receptor Quasi-Immobilization for the Study of Interactions Between Drugs and Serum Albumin","authors":"Xiaoyu Chen,&nbsp;Baian Ji,&nbsp;Meiling Zhou,&nbsp;Hanwen Deng,&nbsp;Min Wang,&nbsp;Zhining Xia","doi":"10.1002/jssc.70142","DOIUrl":"https://doi.org/10.1002/jssc.70142","url":null,"abstract":"<div>\u0000 \u0000 <p>Herein, a receptor quasi-immobilization affinity capillary electrophoresis strategy was developed for the first time, using metal–organic frameworks with bio-macromolecular loading capacity and excellent separation performance, and for the efficient and accurate determination of the interactions between drugs and serum albumin. As a proof-of-concept demonstration, bovine serum albumin was used as the receptor, and zeolitic imidazole framework-8, a metal–organic framework with good biocompatibility and separation performance, was utilized as the chromatographic stationary phase as well as the substrate for the quasi-stationary phase of protein to investigate the interactions between bovine serum albumin and sulfonamides. Relying on the separation capability of the capillary chromatographic column and the extension of the migration time window by the quasi-immobilized receptor, the binding constants between three sulfonamide drugs and bovine serum albumin were successfully determined. The result was sulfadiazine &gt; sulfadimethoxine &gt; sulfaquinoxaline sodium, which was consistent with those obtained by fluorescence spectrometry and traditional affinity capillary electrophoresis. Furthermore, the binding constants of chiral drugs (omeprazole sodium and <span>D</span>, <span>L</span>-tryptophan) with human serum albumin were successfully determined by applying the capillary electrochromatographic column that had been rinsed with acetonitrile solution. In summary, the method not only enables the simultaneous evaluation of interaction between ligands and a protein within a complex system but also allows the investigation of interactions between different biomacromolecules and multicomponent systems through the substitution of quasi-immobilized receptors. Consequently, the present study provides a novel way to facilitate the rapid and accurate screening of active constituents within complex systems.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143856857","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Enantiomeric Resolution of Pharmaceuticals in Capillary Electrophoresis Using Charged and Modified Cyclodextrins: Migration Order, Modeling, and Chiral Resolution Mechanism","authors":"Imran Ali,&nbsp;Ann Gogolashvili,&nbsp;Lali Chankvetadze,&nbsp;Lasha Giunashvili,&nbsp;Hassan Y. Aboul-Enein,&nbsp;Mohamed Hefnawy","doi":"10.1002/jssc.70150","DOIUrl":"https://doi.org/10.1002/jssc.70150","url":null,"abstract":"<div>\u0000 \u0000 <p>The enantiomers of acenocoumarin, coumatetralyl, naproxen, and warfarin were resolved using β-cyclodextrin, 2-hydroxypropyl-β-cyclodextrin, heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin, and heptakis(2,3-di-O-methyl-6-sulfo)-β-cyclodextrin with MES buffer with 0.1% (m/v) hydroxymethyl cellulose as background electrolyte. The migration times and theoretical plates number for R- and S-enantiomers were in the range of 5.08–61.70 and 5.21–65.29 min and 4515–658 045 and 6160–678 976. The values of the selectivity coefficients and resolution factors were 1.02–1.07 and 0.79–4.43, respectively. The enantiomers migration reversal order was determined for the reported racemates. Using a coumatetralyl as an example, the chiral recognition mechanism was determined. The simulation study confirmed the binding energy of R- and S-enantiomers of coumatetralyl as −6.40 and −6.10 kcal/mol; leading R-enantiomer migration first followed by S-enantiomers. The reported methods are useful for the enantiomer ratio of the reported racemates in any unknown samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143850995","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}