Journal of separation science最新文献

{"title":"Next-Generation Chromatography: Covalent Organic Frameworks in Biomedical Analysis","authors":"Kesava Kumar Vudatha,&nbsp;Raja Sundararajan,&nbsp;Lakshmi Vineela Nalla,&nbsp;Siva Nageswara Rao Gajula","doi":"10.1002/jssc.70148","DOIUrl":"https://doi.org/10.1002/jssc.70148","url":null,"abstract":"<p>Chromatography, a cornerstone technique in analytical chemistry, continues to evolve with the emergence of novel stationary phases. Covalent organic frameworks (COFs) have garnered significant attention due to their unique properties and versatile applications. COFs, composed of covalently linked organic building blocks, exhibit high surface area, tunable porosity, and exceptional chemical stability. These attributes make them next-generation chromatographic techniques that leverage novel materials and methodologies to achieve significant improvements in separation efficiency, selectivity, speed, and/or sensitivity compared to traditional methods. COF stationary phases demonstrate remarkable selectivity for small molecules, peptides, proteins, and nucleic acids. Their use in drug discovery, metabolomics, proteomics, and clinical diagnostics is gaining momentum. In this review, we explored their synthesis strategies, emphasizing the design principles that enable tailoring of their physicochemical properties. Further, we discuss the immobilization of COFs onto solid supports, ensuring their compatibility with existing chromatographic systems. Furthermore, we highlighted case studies where COFs outperformed traditional stationary phases, improving sensitivity and resolution. We delve into the integration of COFs as stationary phases in biomedical analysis and explore various strategies for utilizing COFs as stationary phases in chromatographic separations.</p>","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":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70148","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143850994","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":"Electrokinetic Chromatography-based Micro Methods for Separation and Physiochemical Characterization of Very Hydrophobic Pharmaceuticals","authors":"Robert Minkner,&nbsp;Hermann Wätzig","doi":"10.1002/jssc.70127","DOIUrl":"https://doi.org/10.1002/jssc.70127","url":null,"abstract":"<p>This study established an efficient separation of the highly hydrophobic analytes fenofibrate, orlistat, lumefantrine and a micelle marker using microemulsion electrokinetic capillary chromatography. A starting buffer with sodium dodecyl sulphate, heptane and butan-1-ol resulted in a partial separation of the analytes. Various experimental parameters were investigated, including voltage, sample loading time, buffer composition and temperature. An excellent separation was achieved, and compounds with hydrophobicity of up to a calculated log <i>P</i> of 10.2 (est. 12) could be clearly distinguished. Due to observed variabilities in retention time when changing the capillaries, it is advisable to calibrate with a standard mixture before each measurement series.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70127","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143846198","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":"Liquid Chromatographic and Capillary Electromigration Techniques for the Analysis of Azole Antifungals","authors":"Tuuliina Tuominen,&nbsp;Dumidu Perera,&nbsp;Giacomo Russo,&nbsp;Susanne K. Wiedmer","doi":"10.1002/jssc.70135","DOIUrl":"https://doi.org/10.1002/jssc.70135","url":null,"abstract":"<div>\u0000 \u0000 <p>Since the introduction of azoles as antifungals in 1979, they gradually gained a spotlight in both medicinal and industrial fields. Other than being the leading antifungal medicinal drug agents, azoles have also been a major pesticide in agricultural industry. Because of that, numerous amounts of scientific studies have been conducted on azoles using different analytical techniques. Consequently, the requirement to have an in-depth interpretation on the techniques that can successfully be employed has risen. Addressing that, this study reviews analytical research on azole antifungals using liquid chromatography (LC) and capillary electromigration techniques (CE). Sub-techniques within these groups are also considered. Studies performed with CE are reviewed from the year 2015, whereas LC works are reviewed from the year 2020 due to the large number of studies performed by this technique. Emphasis is also placed on chiral separations as these are particularly relevant for azoles as most of them are chiral, and their different enantiomers can exert very different effects on humans and the environment.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143840778","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":"Preparation of Chiral Stationary Phase Co-Modified With Homochiral Secondary Amine Molecular Cages and Amylose and Its Enantiomeric Separation Performance","authors":"Shanshan Sun,&nbsp;Dekuan Hu,&nbsp;Xiaoge Wang,&nbsp;Zhen Li,&nbsp;Guangchuan Ji,&nbsp;Lijun Tang,&nbsp;Hu Zhang,&nbsp;Yimin Zhu,&nbsp;Chen Meng,&nbsp;Jiaxue Chen,&nbsp;Suyu Feng,&nbsp;Lei Yang,&nbsp;Mei Lv,&nbsp;Litao Wang","doi":"10.1002/jssc.70143","DOIUrl":"https://doi.org/10.1002/jssc.70143","url":null,"abstract":"<div>\u0000 \u0000 <p>In this study, reduced porous organic cages with homochiral secondary amine structure were immobilized on a silica gel surface, and a derivative of 3,5-dimethyl phenyl carbamate of amylose was coated onto the molecular cage-modified silica sphere to prepare a chiral stationary phase co-modified with amylose and homochiral secondary amine molecular cages. The prepared chiral stationary phase was characterized using techniques such as scanning electron microscopy, infrared spectroscopy, and thermogravimetric analysis. The results confirmed the successful preparation of the amylose and homochiral secondary amine molecular cages co-modified silica gel chiral stationary phase. The 10 chiral compounds were selected to systematically evaluate the enantioselective performance of the new chiral stationary phase using normal-phase chromatography for enantiomeric separation. The experimental results demonstrated that the 10 compounds were well separated on this chiral stationary phase, with complete separation achieved for trans-stilbene oxide, phenylethanol, and 1-phenyl-1-propanol, all showing a resolution greater than 1.5. In contrast, the homochiral secondary amine molecular cage-modified silica gel stationary phase showed only partial chiral separation for these compounds. The study highlights the synergistic effect of amylose and molecular cages in enhancing enantiomeric separation, demonstrating their significant potential in the development of chiral stationary phases.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143840777","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":"Correction to “Mechanism of Ion Stacking in Aqueous Partition Chromatographic Processes”","authors":"","doi":"10.1002/jssc.70145","DOIUrl":"https://doi.org/10.1002/jssc.70145","url":null,"abstract":"<p>Akter F, Ogiyama Y, Saito S, Shibukawa M. Mechanism of ion stacking in aqueous partition chromatographic processes. <i>J. Sep. Sci</i>. 2017; 40: 3205–3213.</p><p>These errors are only errors in the notation of formulae and have no effect on the manuscript as a whole.</p><p>We apologize for this error.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70145","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143840534","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":"Simultaneous Determination of Eight Bioactive Components of Huangqin Decoction in Rat Plasma by Ultra-high-performance Liquid Chromatography-tandem Mass Spectrometry and Its Application to Comparative Pharmacokinetic Study of Huangqin Decoction in Ulcerative Colitis and Normal Rats","authors":"Xinmiao Tang,&nbsp;Xing Wang,&nbsp;Bo Feng,&nbsp;Yue Cui","doi":"10.1002/jssc.70140","DOIUrl":"https://doi.org/10.1002/jssc.70140","url":null,"abstract":"<div>\u0000 \u0000 <p>Huangqin Decoction (HQD), a traditional Chinese medicine prescription, was first recorded in <i>Treatise on Febrile Diseases</i> 2000 years ago. It is widely used in the treatment of ulcerative colitis (UC). The purpose of the study was to investigate and compare the pharmacokinetic behaviors of the main bioactive components of HQD in UC and normal rats. A simple, rapid, and sensitive liquid chromatography-tandem mass spectrometry method was developed for the simultaneous determination of eight components of HQD in rat plasma. Analytes were separated on a C18 column under gradient elution with a mobile phase consisting of 0.1% formic acid in water and 0.1% formic acid in acetonitrile. Multiple reaction monitoring mode was used to acquire mass transitions. Method validation results showed good specificity and good linearity, with a limit of quantification ranging from 2.5 to 5.0 ng/mL which were sufficient for the pharmacokinetic study. The accuracy and precision were within 12.1% and 11.8%, respectively. Extraction recovery and matrix effect were from 81.8% to 98.8% and 83.6% to 98.4%, respectively. The relative error values of stability under different storage conditions were within 12.8%. The method was successfully applied to study the pharmacokinetics of eight components in UC and normal rat plasma after oral administration of HQD. Pharmacokinetic parameters of analytes were calculated. Results showed that the pharmacokinetic behaviors in UC and normal rats were significantly different, especially time to peak drug concentration (T_max), peak concentration (C_max), and area under the curve (AUC). In general, the C_max of all analytes and AUCs of most analytes in UC rats were markedly lower than in normal rats, which might be related to the pathological state of UC influencing the exposure levels of bioactive components of HQD, and reducing the absorption of them, resulting differences in pharmacokinetic behaviors. This study could provide a reference for the future clinical application of this classical traditional Chinese medicine formula.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143831269","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":"Sustainable Analysis of Diclofenac Salts: A Chemometric Approach to Mixed-Mode Liquid Chromatography With Charged Aerosol Detection","authors":"Bojana Svrkota,&nbsp;Jovana Krmar,&nbsp;Filip Petronijević,&nbsp;Ana Protić,&nbsp;Biljana Otašević","doi":"10.1002/jssc.70136","DOIUrl":"https://doi.org/10.1002/jssc.70136","url":null,"abstract":"<div>\u0000 \u0000 <p>Active pharmaceutical ingredients (APIs) are often used in salt form because of enhanced bioavailability. This study aims to propose a new environmentally friendly method for the analysis of raw diclofenac substance, achieving simultaneous analysis of diclofenac and its counterions (Na⁺ and K⁺), utilizing mixed-mode liquid chromatography (MMLC) and charged aerosol detector (CAD). To optimize the critical method characteristic—the mobile phase composition—a 3² full factorial design of experiments and multiobjective decision making using Derringer's desirability function were employed. Two optimized methods with acceptable run times and satisfactory peak separation were developed. The methods compared the use of acetonitrile (ACN) and acetone (ACE) in terms of method sustainability. The mobile phase composition in the first method (MMLC–ACN) was 40% ACN and 60% ammonium acetate buffer (48.00 mM, pH 4.82), whereas in the second, improved method (MMLC–ACE), it was 50% ACE and 50% ammonium acetate buffer (40.00 mM, pH 4.62). The eco-friendliness of the developed methods was assessed using the GAPI, the Analytical GREEnness (AGREE) score, and the Greenness Index. The method with ACE as the mobile phase modifier demonstrated a better environmental profile, achieving an AGREE score of 0.69, compared to the ACN-based method, which scored 0.60. Method performance characteristics of the MMLC–ACE method used for the quantitative analysis of diclofenac salt raw materials were evaluated according to ICH Q2(R2) guidelines: precision—repeatability (RSD from 1.07% to 2.41% and recovery &gt;97%), selectivity between critical peak pair (<i>α</i>_Na/K &gt; 1) and obtained linear response within concentration range of 50%–150% (<i>r</i> &gt; 0.99).</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143831324","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":"Investigation on the Lipid Profile of Ripened Pu-erh Tea and Relationships Between Their Changes and Key Aromatic Volatiles","authors":"Wenting Li,&nbsp;Lunzhao Yi,&nbsp;Ying Gu,&nbsp;Dabing Ren,&nbsp;Wenjiang Dong","doi":"10.1002/jssc.70133","DOIUrl":"https://doi.org/10.1002/jssc.70133","url":null,"abstract":"<div>\u0000 \u0000 <p>Ripened Pu-erh tea is a special tea with unique flavor and obtained by solid fermentation of microorganisms. This work aimed to investigate the changes of lipid metabolites during fermentation and the association between lipids and the aroma of ripened Pu-erh tea based on ultra-high-performance liquid chromatography-high resolution mass spectrometry and GC-MS. A total of 217 lipids and lipid-soluble substances covering 19 subclasses were detected and characterized. Compared with green tea, black tea, and raw Pu-erh tea, ripened Pu-erh tea showed the highest levels of fatty acids. The contents of 36 lipids varied remarkably with fermentation time, and thus these compounds were screened as differential metabolites. These changes were mainly caused by the degradation of glycerophospholipids (folds change: 0.48–0.13) and the formation of fatty acids (folds change: 5.2–11.2). Results of Pearson correlation analysis showed that a few of the aromatic volatiles, including 2-octenal, 3,5-octadien-2-one, 2,4-heptadienal, and 2,6-nonadienal showed obvious negative correlations with phosphatidylcholine, phosphatidylethanolamine, and phosphatidylinositol, but significant positive correlations with fatty acids 18:2 and 18:1. This study provided a further understanding of the lipid composition of ripened Pu-erh and their changes during tea production.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143826692","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":"Rapid Determination of 25-Hydroxyvitamin D3 and 24,25-Dihydroxyvitamin D3 in Human Urine Based on Polystyrene/Graphene Oxide Packed-Fibers Solid-Phase Extraction Coupled With High-Performance Liquid Chromatography and Atmospheric Pressure Chemical Ionization Tandem Mass Spectrometry","authors":"Qing Han,&nbsp;Min Zhou,&nbsp;Xuejun Kang,&nbsp;Guozhe Deng,&nbsp;Feng Guo,&nbsp;Li Geng","doi":"10.1002/jssc.70130","DOIUrl":"https://doi.org/10.1002/jssc.70130","url":null,"abstract":"<div>\u0000 \u0000 <p>Vitamin D plays a crucial role in skeletal metabolism and is implicated in various diseases. Several studies have indicated that human vitamin D status can be evaluated through urine hydroxyvitamin D levels, in addition to plasma hydroxyvitamin D concentrations. In this study, we developed a novel method for the detection of trace amounts of 25-hydroxyvitamin D₃ [25(OH)D₃] and 24,25-dihydroxyvitamin D₃ [24,25(OH)₂D₃] in urine. This method is based on high-performance liquid chromatography coupled with atmospheric pressure chemical ion source-tandem mass spectrometry, integrated with packed-fibers solid-phase extraction. The composite polystyrene/graphene oxide (PS/GO) nanofibers were synthesized as the sorbent for concentrating 25(OH)D₃ and 24,25(OH)₂D₃, achieving a twentyfold increase in sensitivity when analyzing human urine samples. Fourier-transform infrared spectroscopy, X-ray diffraction, and energy-dispersive X-ray spectroscopy mapping analysis were employed to characterize GO, PS, and PS/GO. The results indicated that the composite nanofibers were successfully synthesized. In addition, we investigated the relationship between the extraction performance of the fibers and the electrospinning process at varying flow rates of spinning solution through morphological studies and Brunauer-Emmett-Teller surface area analysis. During the extraction process, purification, concentration, and desorption were accomplished within a single step. The established method demonstrated excellent sensitivity and efficiency. Under optimal conditions, limits of detection (signal-to-noise ratio = 3) were found to be 0.33 ng/mL for 25(OH)D₃ and 0.19 ng/mL for 24,25(OH)₂D₃; furthermore, linearity was deemed acceptable across urine samples. Recovery rates ranged from 89.5% to 109.7% for 25(OH)D₃ and from 90.3% to 103.1% for 24,25(OH)₂D₃, respectively.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143822324","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":"Preparation and Quaternization of Poly (Styrene-Divinylbenzene) Microspheres Loaded With p-Phenylenediamine-1,3,5-Triformylphloroglucinol Nanoparticles and Utilized as an Anion Exchanger","authors":"Junwei Liu,&nbsp;Haojie Li,&nbsp;Yuqi Yan,&nbsp;Zhaorui Zhang,&nbsp;Yu-an Sun,&nbsp;Guoqing Wang","doi":"10.1002/jssc.70137","DOIUrl":"https://doi.org/10.1002/jssc.70137","url":null,"abstract":"<div>\u0000 \u0000 <p>Covalent organic framework (COF) has been popularly utilized to prepare chromatographic stationary phases due to its a great diversity of composition, unique structure, easy of modification, and so forth. However, the irregular shape and nanometer size scale of most COF materials greatly hinders their direct utilization as chromatographic column packing. Herein, poly (styrene-divinylbenzene) loaded with <i>p</i>-phenylenediamine-1,3,5-triformylphloroglucinol nanoparticles that derived from <i>p</i>-phenylenediamine and 1,3,5-triformylphloroglucinol microspheres are constructed by in situ growth method. Then, the imine groups of poly (styrene-divinylbenzene)@<i>p</i>-phenylenediamine-1,3,5-triformylphloroglucinol are reduced to amino groups and followed by quaternized. The microspheres are characterized by using SEM, Fourier transform infrared spectra, N₂ adsorption-desorption experiment, and so forth. According to the results, poly (styrene-divinylbenzene)@<i>p</i>-phenylenediamine-1,3,5-triformylphloroglucinol microspheres could perfectly combine and possess the good monodispersity of poly (styrene-divinylbenzene) microspheres and unique functionality of <i>p</i>-phenylenediamine-1,3,5-triformylphloroglucinol nanoparticles. The customized column exhibits good separation properties for conventional anions, organic acids, and carbohydrates.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 4","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143818626","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}