Journal of separation science最新文献

{"title":"Adsorption of Rubidium/Cesium From Aqueous Solution Using Silane-Modified Prussian Blue-Based Composites","authors":"Mengmeng Wang,&nbsp;Jian Xu,&nbsp;Liang Zhao,&nbsp;Chenxiao Lin,&nbsp;Jie Gao,&nbsp;Yonggao Xia","doi":"10.1002/jssc.70164","DOIUrl":"https://doi.org/10.1002/jssc.70164","url":null,"abstract":"<div>\u0000 \u0000 <p>This study presents the synthesis and application of a novel silane-modified Prussian blue-based composite (PB-Si) adsorbent for the efficient extraction of rubidium and cesium ions from aqueous solutions. The PB-Si adsorbent is synthesized using the Pickering high internal phase emulsions polymerization method, which leverages the stability of Pickering emulsions formed by nanoparticles at the interface of two immiscible solutions. The modification of Prussian blue with 3-aminopropyl trimethoxy silane enhances the hydrophilicity and stability of the adsorbent. Adsorption kinetics and isotherms results reveal that the PB-Si adsorbent achieves rapid adsorption equilibrium within 2.5–3 h. The PB-Si adsorbent exhibits high adsorption capacities of 317.4 mg/g for Rb⁺ and 402.6 mg/g for Cs⁺. In addition, the developed adsorbent retains 88.3% and 91.7% of its initial adsorption capacity for Rb⁺ and Cs⁺, respectively, after five consecutive adsorption–desorption cycles. The investigation into the adsorption mechanism indicates that chemisorption, driven by electrostatic attraction and chemical complexation with functional groups (─COO⁻) on the surface of the adsorbent, is the dominant process. This study highlights the potential of the PB-Si composite adsorbent as an effective and regenerable material for the extraction of Rb⁺ and Cs⁺ from aqueous solutions, with implications for environmental remediation and resource recovery.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144091589","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":"Evaluation of Analytical Quality by Design Approaches on the Development and Optimization of Size Exclusion Chromatography Analytical Procedures for Bovine Serum Albumin","authors":"Alessio Gaggero,&nbsp;Dalibor Jeremic,&nbsp;Reingard Sattler,&nbsp;Amrit Paudel,&nbsp;Jesús Alberto Afonso Urich","doi":"10.1002/jssc.70168","DOIUrl":"https://doi.org/10.1002/jssc.70168","url":null,"abstract":"<div>\u0000 \u0000 <p>The development of analytical procedures, following the International Council of Harmonisation (ICH) regulatory requirements, is crucial for managing the lifecycle of methodologies. This study applies analytical quality by design (AQbD) principles to optimize size exclusion chromatography (SEC) determination for bovine serum albumin (BSA), chosen as a model drug. Key method variables, including mobile phase buffer concentration, flow rate, and column type, were systematically evaluated using risk assessment and design of experiments (DoE). A consistent and rigorous workflow was applied to prove and ensure the robustness of this methodology. The SEC method was established through a framed analytical target profile (ATP), complying with chromatography parameters like tailing, resolution, capacity, and sensitivity. Those were achieved with a Waters XBridge BEH200A SEC column (200 Å, 3.5 µm, 7.8 mm × 300 mm) at 20°C, using a phosphate buffer saline (PBS) solution at pH 7.4 in isocratic elution with a flow of 0.3 mL/min and UV detection of 280 nm. The method was validated according to ICH Q2 (<i>R</i>²) and Q14 guidelines. The linear response was demonstrated over concentration ranges of 100 µg/mL and 10 mg/mL (<i>R</i>² = 0.9998), and desirable standards of accuracy and precision were met. Although this work highlights the benefits of AQbD in developing trustworthy analytical methods, SEC constitutes a challenge for applying these principles considering the short lifetime of the column, reproducibility, and sensitivity.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949989","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":"Chromatographic Techniques for Improving the LC/MS Quantification of PFAS","authors":"Stephan Buckenmaier,&nbsp;Christina Riemenschneider,&nbsp;Alexander Schächtele,&nbsp;Susanne Sölter","doi":"10.1002/jssc.70155","DOIUrl":"https://doi.org/10.1002/jssc.70155","url":null,"abstract":"<div>\u0000 \u0000 <p>The liquid chromatography / mass spectrometry (LC/MS) quantification of per- and polyfluoroalkyl substances (PFAS) in complex matrices presents challenges. Despite advanced sample preparation techniques to isolate analytes, residual matrix components can still interfere with MS detection. Additionally, extracts often contain high levels of organic solvents limiting the volume that can be injected when using reversed-phase HPLC. Yet, increasing the injection volume could be a simple path to lower detection limits. Feeding PFAS samples, dissolved in pure acetonitrile, at controlled speed into the stream of mobile phase resulted in an analyte focusing effect on the column. By using this approach, the injection volume could be increased 10 times compared to the conventional injection mode, as did the detection sensitivity. Feed injection was coupled to two-dimensional liquid chromatography (2D-LC) in a configuration in which the same triple quadrupole MS could be used for detection in both separation dimensions. The improved separation markedly reduced ion suppression effects and allowed to distinguish the critical PFAS compound perfluorobutanoic acid (PFBA) from isomeric matrix components within tomato extracts interfering with its quantification when only LC/MS was used. This 2D-LC/MS approach therefore fulfilled recommendations that PFBA should be analyzed using a secondary LC approach, without adding a marked amount of time to the analysis.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143944506","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":"Short Review on Currently Used Sample Preparation and Determination Methods of Risdiplam","authors":"Natalia Balińska,&nbsp;Karolina Ostrowska,&nbsp;Sylwia Studzińska","doi":"10.1002/jssc.70173","DOIUrl":"https://doi.org/10.1002/jssc.70173","url":null,"abstract":"<div>\u0000 \u0000 <p>Risdiplam is a new therapeutic agent developed to treat spinal muscular atrophy (SMA), a genetic neurodegenerative disease caused by mutations in the <i>SMN1</i> gene. Unlike previous invasive therapies, risdiplam offers the advantage of oral administration, significantly improving patient comfort and accessibility. The review provides information on an SMA historical overview, breakthrough therapies of the development, and design of the methods used to treat SMA. We then focus on its structure and physicochemical properties. The analysis of risdiplam concentrates on developing improved analytical methods for the precise quantification of risdiplam and its metabolites by high-performance liquid chromatography with mass spectrometry in biological samples using octadecyl stationary phases. For sample preparation, only the protein precipitation method was used. Challenges associated with the risdiplam analytics include developing a highly sensitive and selective method in biological matrices and dealing with potential interferences from the biological matrix. Future research should focus on improving analytical methods, investigating metabolite activity, and expanding our knowledge of its long-term effects.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143938852","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 Analysis of Nine Aromatic Amines in Mainstream Cigarette Smoke Using Modified QuEChERS and Liquid Chromatography–Tandem Mass Spectrometry","authors":"Jie Zhang,&nbsp;Tongguang Xu,&nbsp;Xiang Chang,&nbsp;Ruoshi Bai,&nbsp;Guorong Du,&nbsp;Hongfei Zhang,&nbsp;Dexiang Liu,&nbsp;Zhan Zhang,&nbsp;Jimin Shao,&nbsp;Guangchuan Huang,&nbsp;Jingjing Shang,&nbsp;Yanjun Ma,&nbsp;Chengyong Jiang,&nbsp;Deshui Liu,&nbsp;Nan Lu,&nbsp;Wenwei Li,&nbsp;Yanbo Luo","doi":"10.1002/jssc.70170","DOIUrl":"https://doi.org/10.1002/jssc.70170","url":null,"abstract":"<div>\u0000 \u0000 <p>A modified QuEChERS method coupled with high-performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed to detect nine aromatic amines in mainstream cigarette smoke simultaneously. In this study, a Cambridge filter pad, impregnated with a hydrochloric acid-ethanol solution, was used to trap aromatic amines in vapor and particulate phases in mainstream cigarette smoke. The collection efficiency of aromatic amines for this method was significantly improved compared with conventional methods of trapping aromatic amines using a combination of Cambridge filter pad followed by impinger traps containing dilute acid solution. Utilizing primary secondary amine and C₁₈ for purification effectively removed impurities of different polarities from smoke samples with reduced matrix effect. The limits of detection for the nine aromatic amines were within the range of 0.02–0.10 ng/cig, recoveries were within the range of 86.1%–113.7% and the intraday and interday precisions were both lower than 14%. A collaborative study was conducted involving 10 laboratories to validate developed method for the determination of nine aromatic amines in mainstream cigarette smoke. Statistical evaluation of the results gave good precision results, with an average repeatability relative standard deviation of 5.90%–35.38% and an average reproducibility relative standard deviation of 9.55%–75.72%. As a part of the validation procedure, the developed method was applied to evaluate aromatic amines yields for 17 commercially available cigarettes in China. Compared to the existing methods, this analytical approach affords high sensitivity and efficiency, improved accuracy, and lower cost.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143932356","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":"Maltodextrin-Based Deep Eutectic Solvent as a Chiral Selector for Enantioseparation of Azole Antifungal Drugs in Capillary Electrophoresis","authors":"Wenyang Hu,&nbsp;Hongxia Liu","doi":"10.1002/jssc.70172","DOIUrl":"https://doi.org/10.1002/jssc.70172","url":null,"abstract":"<div>\u0000 \u0000 <p>Deep eutectic solvents have attracted increasing attention in enantioseparation, but only a few studies focus on the development of deep eutectic solvents as the sole chiral selector. In this work, a one-pot synthetic method was used to prepare a deep eutectic solvent based on a polysaccharide chiral selector (maltodextrin) as the sole chiral selector in capillary electrophoresis. Six azole antifungal drugs were used as model drugs to investigate the chiral resolution ability of the maltodextrin-glycerol. Compared to native maltodextrin, the deep eutectic solvents exhibited the more excellent enantioselectivity towards model drugs. Some key factors affecting separation such as maltodextrin concentration, glycerol concentration, buffer pH and separation voltage were investigated. In addition, ultraviolet spectroscopy method and Statistical Product and Service Solutions analysis were adopted to investigate the enhanced chiral recognition mechanism. It is the first time that polysaccharide-based deep eutectic solvents was developed as a favorable chiral selector in capillary electrophoresis, and this research strategy has paved a new way for developing novel chiral materials.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143932378","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":"Benzoyl Chloride Derivatization Coupled With Liquid Chromatography-Mass Spectrometry for the Simultaneous Quantification of Molnupiravir and Its Metabolite β-d-N4-hydroxycytidine in Human Plasma","authors":"Zhilong Yuan,&nbsp;Tao Ma,&nbsp;Lin Xia,&nbsp;Kaile Zheng,&nbsp;Mengdan Liu,&nbsp;Xiujuan Han,&nbsp;Wenjing Zhang,&nbsp;Zhuo Wang","doi":"10.1002/jssc.70162","DOIUrl":"https://doi.org/10.1002/jssc.70162","url":null,"abstract":"<div>\u0000 \u0000 <p>A sensitive and efficient method for simultaneous quantifying molnupiravir and its active metabolite β-<span>d</span>-<i>N</i>⁴-hydroxycytidine in human plasma was developed by combining chemical derivatization with liquid chromatography-tandem mass spectrometry. Through benzoyl chloride chemical derivatization, the analytes exhibited improved mass spectral responses and enhanced chromatographic retention. Besides, the fragmentation patterns were optimized to identify analyte-specific fragments, enhancing detection specificity beyond the common benzoyl fragments. These advancements enabled the method to achieve the lower limits of quantification of 0.4 ng/mL for molnupiravir and 1.0 ng/mL for β-<span>d</span>-<i>N</i>⁴-hydroxycytidine, which represents the lowest reported quantification limits values to date while demonstrating a 30-fold sensitivity enhancement compared to the non-derivatized method under identical instrument conditions. In addition, the sample preparation protocol was streamlined, combining derivatization and sample extraction in a single step, completed within 5 min, eliminating the need for additional handling or reaction time. After undergoing comprehensive validations, the method was successfully applied to clinical samples from patients receiving molnupiravir therapy, demonstrating its practicality for pharmacokinetic monitoring. By combining operational simplicity with sensitivity, this assay provides a reliable tool for advancing research on molnupiravir metabolism and therapeutic drug monitoring.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143932353","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":"Molecularly Imprinted Adsorbent and Its Magnetic Version for Solid Phase Extraction of D-Panthenol: Comparison of Synthesis Approaches, Properties, and Applicability for Different Real Samples Extraction","authors":"Andrea Špačková,&nbsp;Sandra Solčianska-Schwarz,&nbsp;Michaela Kövérová,&nbsp;Izabela Lukačovič Vajová,&nbsp;Radko Tiňo,&nbsp;Katarína Hroboňová","doi":"10.1002/jssc.70161","DOIUrl":"https://doi.org/10.1002/jssc.70161","url":null,"abstract":"<div>\u0000 \u0000 <p>This study demonstrates the development of HPLC-DAD method for determination of D-panthenol incorporating the molecularly imprinted solid-phase extraction for sample preparation. Two types of adsorbents, molecularly imprinted polymers synthesized by bulk polymerization (MIPs) and precipitation polymerization on the surface of magnetic particles (Fe₃O₄@MIP), were compared in terms of adsorption properties and application potential. D-panthenol, a bioactive compound of pharmaceutical and cosmetic products, was used as the template for imprinting. The optimal polymerization mixture included 4-vinylpyridine as the functional monomer and methanol as the porogenic solvent. The adsorption kinetics of the pseudo-second-order indicated chemisorption of the template onto the active sites of the adsorbent. The Freundlich isotherm adsorption model, which fitted experimental data, suggested the presence of heterogeneous sorption sites on the adsorbents. MIPs and Fe₃O₄@MIPs were employed as adsorbents for the solid-phase extraction of D-panthenol from various cosmetic samples (such as body milk and other personal care products) achieving good selectivity for the targeted substance. Recoveries of MIP- and Fe₃O₄@MIP-based extractions were 82.3% (RSD &lt; 2.9%) and 85.8% (RSD &lt; 3.6%), respectively. The proposed HPLC-DAD method exhibited satisfactory linearity over the concentration range of 5.6–100 µg mL⁻¹ (<i>R</i>² = 0.9989) and a limit of detection of 1.7 µg mL⁻¹.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143932357","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":"Deep Eutectic Solvent Extraction Assisted Ligand Affinity Assay for α-Glucosidase Inhibitors Screening From the Plasma of Rats Administrated Pueraria lobata Extracts","authors":"Bing Li,&nbsp;Yidan Lun,&nbsp;Kun Yao,&nbsp;Cheng Tang","doi":"10.1002/jssc.70169","DOIUrl":"https://doi.org/10.1002/jssc.70169","url":null,"abstract":"<div>\u0000 \u0000 <p>In this work, for the first time, a deep eutectic solvent assisted ligand affinity assay was proposed. Several critical parameters affecting the analysis performance were investigated and the optimized DES extract conditions were as follows: the solution of tetrabutylammonium chloride–ethylene glycol (1:2) was prepared as an extract solution. A total of 1.4 mol/L sodium citrate (pH = 6.6) was used for phase separation, and the vortex extraction time was 5 min. Analytes could be enriched in the phase of deep eutectic solvent after phase separation. Then, they could be analyzed by α-glucosidase immobilized magnetic beads affinity assay directly. Results showed the proposed method could detect luteolin (a positive control) from plasma selectively. The LOD was 2 µg/mL. The intraday precision and the interday precision were 7.86% and 6.66%, respectively. By using the proposed method as a tool, plasma of the rats that administrated the extract of <i>Pueraria lobata</i> was analyzed. The bio-active flavonoids absorbed in the body such as puerarin, daidzin, daidzein, and a metabolite of puerarin (puerarin glucuronide) were found. The method has the benefits of a simplified analytic process, high resolution, and is a reliable method.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143932377","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":"Quantification of Epigenetic DNA and RNA Modifications by UHPLC–MS/MS Technologies: New Concepts and New Improvements for the Special Collections","authors":"Rui Zhang,&nbsp;Hailong Liu,&nbsp;Biao Bai,&nbsp;Hailin Wang","doi":"10.1002/jssc.70159","DOIUrl":"https://doi.org/10.1002/jssc.70159","url":null,"abstract":"<div>\u0000 \u0000 <p>Dynamic and reversible DNA and RNA modifications are essential for cell differentiation and development. Aberrant epigenetic modifications are closely associated with the occurrence and progression of diseases, serving as potential markers for cancer diagnosis and prognosis. Ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS) offers distinct advantages in the qualitative and quantitative analysis of various modifications due to its sensitivity, specificity, and accuracy. This review provides a comprehensive overview of the current knowledge regarding the liquid chromatography–mass spectrometry (LC–MS) analysis of DNA and RNA modifications, including analytical procedures, advancements, and biological applications, with a focus on tracing the source of (N6-2′-deoxy-adenosine) 6mdA in eukaryotes. Additionally, we examine the integration of UHPLC–MS/MS with other separation techniques to achieve accurate quantification of modifications in specific regions, certain fragments, and free nucleosides.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143925973","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}