Lu Zhang, Xujia Cai, Yongzhe Cheng, Shiyi Chen, Min Zhang, Hongyang Zhang, Ping Hu
{"title":"Chemical Profiling and Quality Evaluation of Gualou-Xiebai Herbal Pair by Liquid Chromatography-Tandem Mass Spectrometry With Feature-Based Molecular Network and High-Performance Liquid Chromatography With Charged Aerosol Detector","authors":"Lu Zhang, Xujia Cai, Yongzhe Cheng, Shiyi Chen, Min Zhang, Hongyang Zhang, Ping Hu","doi":"10.1002/jssc.70108","DOIUrl":"https://doi.org/10.1002/jssc.70108","url":null,"abstract":"<div>\u0000 \u0000 <p>Gualou-Xiebai (GX), a traditional Chinese herbal pair, is often used in the treatment of cardiovascular diseases. However, the investigation into the components of GX is not comprehensive enough. In order to obtain the chemical profile of GX, a method that combined mass spectrometry with a feature-based molecular network was utilized for the identification of its complex constituents. In total, 121 compounds were annotated and four potential new compounds were inferred. In addition, an optimized fingerprint analysis method using high-performance liquid chromatography coupled with a charged aerosol detector was established, which was further validated and implemented for the simultaneous quantification of 17 ingredients in GX, including the semi-quantitative analysis of 13 allium saponins and the quantitative analysis of four fatty acids. This method achieved the detection of no ultraviolet absorption constituents in GX. The results have an important impact on revealing the chemical basis of GX and lay a foundation for further quality assessment.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 3","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143521801","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}
Yan Zhao, Huaming Sun, Hongxia Yu, Thi Hong Van Le, Xiuheng Qin, Xiaodi Dong, Guiyun Cao, Zhaoqing Meng, Zheng Wang, Ammara Sohail, Jeonghill Park, Daijie Wang
{"title":"An Efficient Method to Separate the Main Components from Black Ginseng of Panax quinquefolium L. by Recycling and Consecutive High-Speed Counter-Current Chromatography Coupled With Evaporative Light Scattering Detection","authors":"Yan Zhao, Huaming Sun, Hongxia Yu, Thi Hong Van Le, Xiuheng Qin, Xiaodi Dong, Guiyun Cao, Zhaoqing Meng, Zheng Wang, Ammara Sohail, Jeonghill Park, Daijie Wang","doi":"10.1002/jssc.70105","DOIUrl":"https://doi.org/10.1002/jssc.70105","url":null,"abstract":"<div>\u0000 \u0000 <p>Black ginseng (BG), a novel manufactured ginseng product, is gaining market attention due to its high polarity and similar structure constituents. In this work, the primary constituents of <i>Panax quinquefolium</i> L. BG, including ginsenosides and derivatives, were separated using high-speed counter-current chromatography in conjunction with evaporative light scattering detection by recycling and consecutive mode, as well as the elution-extrusion method for continuous sample loading. Sample loading and mobile phase ratios were among the optimized primary separation parameters. Nine compounds, including ginsenoside Rg6 (<b>1</b>), 22(<i>E</i>)-ginsenoside F4 (<b>2</b>), ginsenoside Rk3 (<b>3</b>), ginsenoside Rh4 (<b>4</b>), ginsenoside Rg3 (<b>5</b>), 20(<i>R</i>)-ginsenoside Rg3 (<b>6</b>), (3<i>R</i>,9<i>R</i>,10<i>R</i>)-panaxytriol (<b>7</b>), ginsenoside Rk1 (<b>8</b>), and ginsenoside Rg5 (<b>9</b>), were ultimately effectively isolated. Mass spectrometry and nuclear magnetic resonance spectrometry were used to investigate the structures. Based on our research, the developed process was a successful way to separate the primary ingredients from BG. Purification of additional comparable high-polarity chemicals from complicated natural products might be accomplished using the stated methodology.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 3","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143521800","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":"Fractionation and Characterization of Humic Substances in Nutritional Supplements Using Immobilized Metal Affinity Chromatography","authors":"Radoslav Halko, Róbert Góra, Massoud Kaykhaii","doi":"10.1002/jssc.70104","DOIUrl":"https://doi.org/10.1002/jssc.70104","url":null,"abstract":"<div>\u0000 \u0000 <p>This work presents the study of the immobilized metal affinity chromatography method for the analysis of humic substances in a few food supplements. Separation mechanisms of the immobilized metal affinity chromatography method are based on the affinity of functional groups of humic substances to metal ions. The immobilized metal affinity chromatography system employed an Iontosorb Salicyl sorbent with immobilized aluminum ions. A step-wise gradient was used for elution, consisting of two mobile phases of acetate buffer solution at varying pH values and a mixture of sulfuric acid and sodium sulfate. The change in concentration and volume of Al(III) ions and pH of the eluent have been studied for sorption characteristics and immobilized metal affinity chromatography separation. The chosen value was 0.20 mmol of aluminum per 1 g of the chelating sorbent at pH 7.0. The immobilized metal affinity chromatography system has been studied by using a pair of substances with different chelating properties (phenol and salicylic acid) and a mixture of eleven substances, which represented a simplified model structure of humic substances. The results of these studies have been applied to the fractionation of humic substance standards and to the characterization of humic substances in food supplements containing humic substances by the immobilized metal affinity chromatography system. To better characterize particular humic substances, the immobilized metal affinity chromatography fractions were further analyzed by size-exclusion chromatography. Based on the results obtained, the immobilized metal affinity chromatography method appears to be a promising tool for the analysis of humic substances, and it may help in the characterization of their structure and understanding their interactions with metal ions.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 3","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143521802","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":"Determination of Mitragynine and 7-Hydroxymitragynine in Raw Kratom Plant Material by a Multisegment Injection Capillary Zone Electrophoresis-Tandem Mass Spectrometry","authors":"Andrea Horniakova, Peter Mikus, Juraj Piestansky","doi":"10.1002/jssc.70106","DOIUrl":"https://doi.org/10.1002/jssc.70106","url":null,"abstract":"<div>\u0000 \u0000 <p>A novel validated analytical approach implementing multisegment injection strategy into the capillary zone electrophoresis-tandem mass spectrometry hyphenation for determination of two psychoactive alkaloids, mitragynine (MIT), and 7-hydoxymitraginine (7-OH-MIT), in kratom raw samples was introduced. A thorough optimization of the multisegment injection strategy and extraction procedure of the alkaloids from raw powdered plant material was realized. The separation of the two secondary plant metabolites was performed in the background electrolyte composed of 100 mM formic acid. The developed and optimized analytical approach showed favorable operation and validation parameters, including linearity (<i>r</i><sup>2</sup> > 0.99), selectivity, precision (relative standard deviation in the range of 3.3%–9.4%), accuracy (relative error in the range of 92.2%–108.4%), recovery (85.1%–99.7%), or robustness (95.2%–99.7%). Furthermore, the method demonstrates high sensitivity, with the limit of detection at the concentration level of 1 and 2 ng/mL for MIT and 7-hydroxymitragynine, respectively. Finally, the method was successfully applied to determine the content of the psychoactive alkaloids in six raw kratom samples marketed as collector's items. The content of MIT and 7-OH-MIT in the kratom samples (original powdered raw material) varied from 23.15 to 35.51 and 0.43 to 0.72 µg/mg, respectively. Moreover, the developed innovative approach was assessed to evaluate sample preparation sustainability, alignment with green analytical chemistry principles, and practicality. The proposed method with enhanced sample throughput represents a very effective and promising green alternative to traditional chromatographic techniques and has high potential for implementation in pharmaceutical and toxicological practice.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 3","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143513556","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":"Recent Advance in the Synthesis and Applications of Chiral Covalent Organic Frameworks: A Mini-Review","authors":"Qiuyi Liu, Zhu Li, Jing Sun, Yue Lan, Jiaqi Hu, Yuqiang Xiao, Feng-Qing Yang, Die Gao","doi":"10.1002/jssc.70101","DOIUrl":"https://doi.org/10.1002/jssc.70101","url":null,"abstract":"<div>\u0000 \u0000 <p>Chiral covalent organic frameworks (CCOFs) are emerging porous materials with tunable chiral structures, abundant pores, and high surface areas, gaining significant attentions in separation, sensing, and asymmetric catalysis. This review summarizes the synthesis methods of CCOFs and their applications in chiral recognition. It discusses the advantages and limitations of three synthesis strategies, including chiral post-modification, direct synthesis, and chiral-induced synthesis. The review also highlights the potential of CCOFs in chiral separation, sensing, and asymmetric catalysis for efficient purification, detection, and synthesis of chiral molecules. Challenges and future directions for the preparation and application of CCOFs are also addressed, aiming to guide further research and practical applications.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143466269","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":"Separation, Analysis, and Degradation of Cembranoids in Flue-Cured Tobacco Leaves","authors":"Yue Xie, Kailong Yuan, Junchen Zhu, Yonggang Zhang, Xiaobing Zhang, Hongru Feng, Yuanjiang Pan, Cuirong Sun","doi":"10.1002/jssc.70103","DOIUrl":"https://doi.org/10.1002/jssc.70103","url":null,"abstract":"<div>\u0000 \u0000 <p>Cembranoids are significant flavor precursors found in flue-cured tobacco leaves. The degradation products can serve as important aromatic compounds. In this study, 16 cembranoids were discovered in flue-cured tobacco leaves by liquid chromatography–mass spectrometry (MS), and 1 cembranoid featuring both oxidation and dehydrogenation from α<i>/</i>β-cembranoid was identified for the first time. α- and β-cembranoids were confirmed to be precursors to various degradation products. Additionally, β-cembranoid was prone to epimerize into α-cembranoid while simultaneously undergoing allylic rearrangement, with the hydroxyl group undergoing migration. During the aging and curing processes, cembranoids can easily add oxygen atoms to the carbon–carbon double bonds, whereas the hydroxyl group in the structure may form epoxides, oxidize into ketones, or undergo dehydration reactions. Additionally, the microwave plasma torch interfaced with an MS was used to create and detect the pyrolysis and oxidized products of cembranoids. More degradation products were discovered, including oxidation products with the addition of one to three oxygen atoms, as well as a series of aromatic compounds such as 1,3,5-heptatriene and its range of homologs. This research presented the different degradation pathways of cembranoids in flue-cured tobacco during aging and curing processes, offering valuable insights for the enhancement of tobacco production techniques and quality control.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143466267","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":"Separation, Analysis, and Degradation of Cembranoids in Flue-Cured Tobacco Leaves","authors":"Yue Xie, Kailong Yuan, Junchen Zhu, Yonggang Zhang, Xiaobing Zhang, Hongru Feng, Yuanjiang Pan, Cuirong Sun","doi":"10.1002/jssc.70103","DOIUrl":"https://doi.org/10.1002/jssc.70103","url":null,"abstract":"<div>\u0000 \u0000 <p>Cembranoids are significant flavor precursors found in flue-cured tobacco leaves. The degradation products can serve as important aromatic compounds. In this study, 16 cembranoids were discovered in flue-cured tobacco leaves by liquid chromatography–mass spectrometry (MS), and 1 cembranoid featuring both oxidation and dehydrogenation from α<i>/</i>β-cembranoid was identified for the first time. α- and β-cembranoids were confirmed to be precursors to various degradation products. Additionally, β-cembranoid was prone to epimerize into α-cembranoid while simultaneously undergoing allylic rearrangement, with the hydroxyl group undergoing migration. During the aging and curing processes, cembranoids can easily add oxygen atoms to the carbon–carbon double bonds, whereas the hydroxyl group in the structure may form epoxides, oxidize into ketones, or undergo dehydration reactions. Additionally, the microwave plasma torch interfaced with an MS was used to create and detect the pyrolysis and oxidized products of cembranoids. More degradation products were discovered, including oxidation products with the addition of one to three oxygen atoms, as well as a series of aromatic compounds such as 1,3,5-heptatriene and its range of homologs. This research presented the different degradation pathways of cembranoids in flue-cured tobacco during aging and curing processes, offering valuable insights for the enhancement of tobacco production techniques and quality control.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143466270","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":"Recent Advance in the Synthesis and Applications of Chiral Covalent Organic Frameworks: A Mini-Review","authors":"Qiuyi Liu, Zhu Li, Jing Sun, Yue Lan, Jiaqi Hu, Yuqiang Xiao, Feng-Qing Yang, Die Gao","doi":"10.1002/jssc.70101","DOIUrl":"https://doi.org/10.1002/jssc.70101","url":null,"abstract":"<div>\u0000 \u0000 <p>Chiral covalent organic frameworks (CCOFs) are emerging porous materials with tunable chiral structures, abundant pores, and high surface areas, gaining significant attentions in separation, sensing, and asymmetric catalysis. This review summarizes the synthesis methods of CCOFs and their applications in chiral recognition. It discusses the advantages and limitations of three synthesis strategies, including chiral post-modification, direct synthesis, and chiral-induced synthesis. The review also highlights the potential of CCOFs in chiral separation, sensing, and asymmetric catalysis for efficient purification, detection, and synthesis of chiral molecules. Challenges and future directions for the preparation and application of CCOFs are also addressed, aiming to guide further research and practical applications.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143466268","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}
Maria Kousi, Natasa P. Kalogiouri, Victoria F. Samanidou
{"title":"Recent Advances in Bioanalysis of Cephalosporins Toward Green Sample Preparation","authors":"Maria Kousi, Natasa P. Kalogiouri, Victoria F. Samanidou","doi":"10.1002/jssc.70096","DOIUrl":"https://doi.org/10.1002/jssc.70096","url":null,"abstract":"<p>This review highlights recent advances in the bioanalysis of cephalosporins using liquid chromatographic methods, focusing on green sample preparation (GSP) techniques. Cephalosporins, a class of β-lactam antibiotics, are critical in combating bacterial infections but present challenges related to drug resistance and toxicity. This article evaluates various sample preparation methods, including solid-phase extraction, solid-phase microextraction, and protein precipitation, which have been employed in the extraction and quantification of cephalosporins from biological matrices. Special attention is given to the optimization of critical parameters, such as pH, extraction solvents, and purification techniques to maximize analytes’ recovery and sensitivity. Emerging trends in GSP, such as the use of molecularly imprinted polymers and miniaturized processing devices, are also discussed. The review underscores the growing importance of integrating environmentally friendly approaches in cephalosporin bioanalysis, paving the way for future innovations in bioanalytical research.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70096","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143446937","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}
Maria Kousi, Natasa P. Kalogiouri, Victoria F. Samanidou
{"title":"Recent Advances in Bioanalysis of Cephalosporins Toward Green Sample Preparation","authors":"Maria Kousi, Natasa P. Kalogiouri, Victoria F. Samanidou","doi":"10.1002/jssc.70096","DOIUrl":"https://doi.org/10.1002/jssc.70096","url":null,"abstract":"<p>This review highlights recent advances in the bioanalysis of cephalosporins using liquid chromatographic methods, focusing on green sample preparation (GSP) techniques. Cephalosporins, a class of β-lactam antibiotics, are critical in combating bacterial infections but present challenges related to drug resistance and toxicity. This article evaluates various sample preparation methods, including solid-phase extraction, solid-phase microextraction, and protein precipitation, which have been employed in the extraction and quantification of cephalosporins from biological matrices. Special attention is given to the optimization of critical parameters, such as pH, extraction solvents, and purification techniques to maximize analytes’ recovery and sensitivity. Emerging trends in GSP, such as the use of molecularly imprinted polymers and miniaturized processing devices, are also discussed. The review underscores the growing importance of integrating environmentally friendly approaches in cephalosporin bioanalysis, paving the way for future innovations in bioanalytical research.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 2","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70096","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143446936","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}