Journal of separation science最新文献

{"title":"Comprehensive Quality Evaluation of Viticis Fructus Based on Simultaneous Quantification of Nine Flavones and One Iridoid Glycoside by Ultra-High Performance Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry and Chemometric Analysis","authors":"Wen-Jing Ren,&nbsp;Yi-Zhe Liu,&nbsp;Rezeye Aili,&nbsp;Zhao-Xia Li,&nbsp;Feng Qiu","doi":"10.1002/jssc.70174","DOIUrl":"https://doi.org/10.1002/jssc.70174","url":null,"abstract":"<div>\u0000 \u0000 <p>Viticis fructus is the dry fruit of <i>Vitex trifolia</i> L. var. <i>simplicifolia</i> Cham. or <i>Vitex trifolia</i> L., both belonging to the family Verbenaceae. Viticis fructus can grow well in saline alkali lands, and is currently an important industrial raw material for extracting flavones and iridoid glycosides for medicinal use. However, the significance of differences in the chemical components of Viticis fructus from different production areas is not yet clear. Therefore, a sensitive, selective, and accurate UHPLC–ESI–MS/MS method with high selectivity and efficiency was established and validated for simultaneous quantification of nine flavones and one iridoid glycoside in Viticis fructus. A comprehensive quality evaluation of 36 batches of Viticis fructus samples collected from 10 main production areas in China was performed using this method and chemometric analysis. The contents of vitexicarpin in 36 batches of samples were all higher than 0.030% (300 µg/g), which met the requirements of <i>Chinese Pharmacopoeia</i> (2020 edition). However, the contents of the 10 active ingredients from different production areas were quite different. The contents of nine flavones and one iridoid glycoside in Viticis fructus were greatly affected by the growth environment. Humid climatic conditions were relatively favorable for the accumulation of active components in Viticis fructus. The flavone and iridoid glycoside contents were higher in the samples from Shandong, Jiangxi, Guangxi, and Guizhou. Chemometric analysis also showed that vitexicarpin, chrysosplenol D, and agnuside could well represent the total flavones and iridoid glycoside of Viticis fructus for the classification and evaluation of the overall quality of Viticis fructus from different regions. These three representative components can be used as markers to evaluate the quality of Viticis fructus, providing a reliable theoretical and experimental basis for improving the quality standards of Viticis fructus.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144220067","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":"Covalent/Metal–Organic Skeleton Composites for Solid-Phase Extraction of Ultraviolet Absorbers in Environmental Samples","authors":"Mengxi Li,&nbsp;Xinrui Tian,&nbsp;Jiayi Song,&nbsp;Ping Su,&nbsp;Yi Yang","doi":"10.1002/jssc.70186","DOIUrl":"https://doi.org/10.1002/jssc.70186","url":null,"abstract":"<div>\u0000 \u0000 <p>In this study, novel covalent/metal–organic skeleton composites (TpBD@MIL-68; 2,4,6-triformylphloroglucinol (Tp) and benzidine (BD)) were combined with high-performance liquid chromatography (HPLC) and used to develop a method for detecting ultraviolet absorbers, including 4-(4,6-diphenyl-1,3,5-triazin-2-yl)benzene-1,3-diol (Appolo-116), 3-benzenediol, 4-[4,6-bis(2,4-dimethylphenyl)-1,3,5-triazin-2-yl]-1 (DBDT), 2,4,6-triphenyl-s-triazine (TPTZ), 2,4,6-trip-tolyl-1.3.5-triazine, 2-(4,6-diphenyl-1,3,5-triazin-2-yl)-5-((hexyl)oxy)phenol (UV-1577), and 2-(4,6-bis-(2,4-dimethylphenyl)-1,3,5-triazin-2-yl)-5-(octyloxy)-phenol (UV-1164) is present in greenhouse films and soils. TpBD@MIL-68 has the unique characteristics of a covalent organic framework and a metal–organic framework. TpBD@MIL-68 exhibited a higher extraction efficiency because of π–π and electrostatic interactions between the benzene ring structure of the TpBD, MIL-68, and the ultraviolet absorber molecules. The extraction conditions, including the adsorbent dosage, eluent type and dosage, elution time, and the pH of the sample solution, were fully optimized. The extraction efficiency of TpBD@MIL-68 exceeded 80%. The detection results showed good linearity over a wide range of concentrations (5–5000 µg/L) and low detection limits (0.61–0.94 ng/mL) for target molecules. The practicability of this solid-phase extraction (SPE)–HPLC method was further evaluated by analyzing greenhouse films and soils, with target recoveries of 80.9%–109.9% and relative standard deviations of less than 8.9%. The as-synthesized TpBD@MIL-68 adsorbent exhibited great potential in ultraviolet absorber analysis.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144220070","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":"Performance of the Reverse Fill/Flush Flow Modulation With Tunable Auxiliary Forward-Pressure Control in the Conditions When the Second Gas Chromatography Column Outlet Pressure Is Different From the Atmospheric Pressure","authors":"Aleksandra Lelevic","doi":"10.1002/jssc.70182","DOIUrl":"https://doi.org/10.1002/jssc.70182","url":null,"abstract":"<div>\u0000 \u0000 <p>Reverse fill/flush flow modulation is an effective approach for peak modulation in comprehensive two-dimensional gas chromatography, and several homemade or commercial solutions have been demonstrated. In terms of configuration, systems with either a fixed bleed capillary or tunable forward or back pressure regulation permit to effectively maintain an optimal modulator channel flow and good modulation performance. In both cases, however, in the up-to-date reported works, the modulator channel flow regulation conditions remain constant during the GC run. In this work it was shown that if the objective is to maintain a constant modulator channel flow, constant pressure–resistance regulation conditions can be an issue when the secondary gas chromatography column outlet pressure is not equal to the outlet pressure of the bleed capillary. When the secondary column outlet is connected to a detector, such as, for example, VUV, or to a purged splitter where an elevated constant pressure is applied, which were both tested in this study, in these cases the temperature changes during the GC run impose having to vary the chosen pressure resistance conditions for maintaining a constant modulator channel flow. It was shown, however, that modulator channel flow variation during the GC run appeared minimal when a fixed bleed capillary was used but increased significantly if a tunable auxiliary flow of carrier gas was rather employed. In addition, it was demonstrated through theoretical calculations and experiments that the temperature dependence of the auxiliary carrier gas flow necessary for maintaining a certain constant modulator channel flow is not linear but rather closer to a second-degree polynomial. While a linear approximation can be sufficient in some cases, in other cases the modulation performance can be impacted more significantly, and thus auxiliary carrier gas flow programming according to a second-degree polynomial model can be preferred.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144197046","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":"Purification of Pharmaceuticals via Retention Time Prediction: Leveraging Graph Isomorphism Networks, Limited Data, and Transfer Learning","authors":"Armen G. Beck,&nbsp;Rojan Shrestha,&nbsp;Jun Wang,&nbsp;Jonathan Fine,&nbsp;Erik L. Regalado,&nbsp;Kanaka Hettiarachchi,&nbsp;Katharine B. Williams,&nbsp;Edward C. Sherer,&nbsp;Pankaj Aggarwal","doi":"10.1002/jssc.70178","DOIUrl":"https://doi.org/10.1002/jssc.70178","url":null,"abstract":"<div>\u0000 \u0000 <p>The design-make-test cycle for drug discovery is highly dependent on the purification of synthesized compounds. Prior to evaluation of suitability, ultrahigh-performance liquid chromatography is used for an initial standard analysis, where retention times of analytes are measured with a shorter standard gradient method and used to select the appropriate gradients for a final purification method. To circumvent this preliminary screening experiment for small molecule libraries, retention time prediction had been achieved previously by the use of commercial modeling methods. However, these retention time prediction models can have limited applicability when built from smaller datasets and are less effective when constructed from disparate data collected under differing chromatography conditions. Having thousands of measured retention times from high-throughput physiochemical screening, we sought to leverage these data for the construction of predictive models for a standard preliminary method enabling high-throughput purification of macrocyclic peptide libraries. Utilizing 4549 analytes and their retention times from high-throughput physiochemical screening, a structure-to-retention-time model was built using a graph isomorphism network, a form of artificial neural network architecture. Once fitted to high-throughput screening data, the model was re-trained with standard gradient method data, a technique known as transfer learning. Through transfer learning, a training set of 80 analytes yielded a neural network model that, when evaluated against a test set of 24 analytes, displays high performance metrics with a coefficient of determination (<i>R</i>²) of 0.82 and mean average error of 0.088 min, or 1.26% of the gradient time. Comparatively, the best commercial quantitative structure-retention relationship model poorly performed, with an <i>R</i>² of 0.11 and mean average error of 0.202 min. This model has been deployed internally as a Dash app to help democratize the use of the developed models and is being used for selecting purification methods based on analyte structure.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144197127","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":"The Reverse Molecular Assembly Analysis Strategy for Rapid Discovery of Potential New Compounds in Codonopsis Radix Based on UHPLC-Q-Exactive Orbitrap MS/MS","authors":"Shuteng Huang,&nbsp;Hanxiu Deng,&nbsp;Shuyi Song,&nbsp;Xianming Lan,&nbsp;Hongyan Zhou,&nbsp;Qinqing Li,&nbsp;Jiayu Zhang","doi":"10.1002/jssc.70181","DOIUrl":"https://doi.org/10.1002/jssc.70181","url":null,"abstract":"<div>\u0000 \u0000 <p>Deciphering the chemical basis of traditional Chinese medicine (TCM) is of far-reaching significance for revealing its pharmacodynamic mechanism, metabolic transformation, and drug development. However, the complexity of chemical compositions and the large number of isomers in TCM make it difficult to achieve comprehensive detection and identification. Taking <i>Codonopsis</i> Radix as a case, we proposed a reverse molecular assembly (RMA) analysis strategy for rapid discovery of potential new compounds in the complex system of TCM: the paired diagnostic product ions (pDPIs) were designed based on the structural characteristics and characteristic cleavage pathways of taxa-compounds. First, the reported compounds were categorized into different taxa based on different core structures. Second, pDPIs belonging to a certain taxon were designed according to different core structures, branch chains, and cleavage pathways. Third, the accuracy of pDPIs in positive and negative ion modes was verified by comparing mass spectrometry data, literature reports, and standards. Finally, the RMA analysis strategy was used to accurately identify the chemical components of <i>Codonopsis</i> Radix extract. In this study, 209 compounds were preliminarily characterized, 128 of which are potential new compounds that have not been reported yet in <i>Codonopsis</i> Radix. This study provides an important reference for in-depth elucidation of the chemical basis of the complex system of TCM.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144197129","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":"The Reverse Molecular Assembly Analysis Strategy for Rapid Discovery of Potential New Compounds in Codonopsis Radix Based on UHPLC-Q-Exactive Orbitrap MS/MS","authors":"Shuteng Huang,&nbsp;Hanxiu Deng,&nbsp;Shuyi Song,&nbsp;Xianming Lan,&nbsp;Hongyan Zhou,&nbsp;Qinqing Li,&nbsp;Jiayu Zhang","doi":"10.1002/jssc.70181","DOIUrl":"https://doi.org/10.1002/jssc.70181","url":null,"abstract":"<div>\u0000 \u0000 <p>Deciphering the chemical basis of traditional Chinese medicine (TCM) is of far-reaching significance for revealing its pharmacodynamic mechanism, metabolic transformation, and drug development. However, the complexity of chemical compositions and the large number of isomers in TCM make it difficult to achieve comprehensive detection and identification. Taking <i>Codonopsis</i> Radix as a case, we proposed a reverse molecular assembly (RMA) analysis strategy for rapid discovery of potential new compounds in the complex system of TCM: the paired diagnostic product ions (pDPIs) were designed based on the structural characteristics and characteristic cleavage pathways of taxa-compounds. First, the reported compounds were categorized into different taxa based on different core structures. Second, pDPIs belonging to a certain taxon were designed according to different core structures, branch chains, and cleavage pathways. Third, the accuracy of pDPIs in positive and negative ion modes was verified by comparing mass spectrometry data, literature reports, and standards. Finally, the RMA analysis strategy was used to accurately identify the chemical components of <i>Codonopsis</i> Radix extract. In this study, 209 compounds were preliminarily characterized, 128 of which are potential new compounds that have not been reported yet in <i>Codonopsis</i> Radix. This study provides an important reference for in-depth elucidation of the chemical basis of the complex system of TCM.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144197049","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":"Performance of the Reverse Fill/Flush Flow Modulation With Tunable Auxiliary Forward-Pressure Control in the Conditions When the Second Gas Chromatography Column Outlet Pressure Is Different From the Atmospheric Pressure","authors":"Aleksandra Lelevic","doi":"10.1002/jssc.70182","DOIUrl":"https://doi.org/10.1002/jssc.70182","url":null,"abstract":"<div>\u0000 \u0000 <p>Reverse fill/flush flow modulation is an effective approach for peak modulation in comprehensive two-dimensional gas chromatography, and several homemade or commercial solutions have been demonstrated. In terms of configuration, systems with either a fixed bleed capillary or tunable forward or back pressure regulation permit to effectively maintain an optimal modulator channel flow and good modulation performance. In both cases, however, in the up-to-date reported works, the modulator channel flow regulation conditions remain constant during the GC run. In this work it was shown that if the objective is to maintain a constant modulator channel flow, constant pressure–resistance regulation conditions can be an issue when the secondary gas chromatography column outlet pressure is not equal to the outlet pressure of the bleed capillary. When the secondary column outlet is connected to a detector, such as, for example, VUV, or to a purged splitter where an elevated constant pressure is applied, which were both tested in this study, in these cases the temperature changes during the GC run impose having to vary the chosen pressure resistance conditions for maintaining a constant modulator channel flow. It was shown, however, that modulator channel flow variation during the GC run appeared minimal when a fixed bleed capillary was used but increased significantly if a tunable auxiliary flow of carrier gas was rather employed. In addition, it was demonstrated through theoretical calculations and experiments that the temperature dependence of the auxiliary carrier gas flow necessary for maintaining a certain constant modulator channel flow is not linear but rather closer to a second-degree polynomial. While a linear approximation can be sufficient in some cases, in other cases the modulation performance can be impacted more significantly, and thus auxiliary carrier gas flow programming according to a second-degree polynomial model can be preferred.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144197050","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":"Purification of Pharmaceuticals via Retention Time Prediction: Leveraging Graph Isomorphism Networks, Limited Data, and Transfer Learning","authors":"Armen G. Beck,&nbsp;Rojan Shrestha,&nbsp;Jun Wang,&nbsp;Jonathan Fine,&nbsp;Erik L. Regalado,&nbsp;Kanaka Hettiarachchi,&nbsp;Katharine B. Williams,&nbsp;Edward C. Sherer,&nbsp;Pankaj Aggarwal","doi":"10.1002/jssc.70178","DOIUrl":"https://doi.org/10.1002/jssc.70178","url":null,"abstract":"<div>\u0000 \u0000 <p>The design-make-test cycle for drug discovery is highly dependent on the purification of synthesized compounds. Prior to evaluation of suitability, ultrahigh-performance liquid chromatography is used for an initial standard analysis, where retention times of analytes are measured with a shorter standard gradient method and used to select the appropriate gradients for a final purification method. To circumvent this preliminary screening experiment for small molecule libraries, retention time prediction had been achieved previously by the use of commercial modeling methods. However, these retention time prediction models can have limited applicability when built from smaller datasets and are less effective when constructed from disparate data collected under differing chromatography conditions. Having thousands of measured retention times from high-throughput physiochemical screening, we sought to leverage these data for the construction of predictive models for a standard preliminary method enabling high-throughput purification of macrocyclic peptide libraries. Utilizing 4549 analytes and their retention times from high-throughput physiochemical screening, a structure-to-retention-time model was built using a graph isomorphism network, a form of artificial neural network architecture. Once fitted to high-throughput screening data, the model was re-trained with standard gradient method data, a technique known as transfer learning. Through transfer learning, a training set of 80 analytes yielded a neural network model that, when evaluated against a test set of 24 analytes, displays high performance metrics with a coefficient of determination (<i>R</i>²) of 0.82 and mean average error of 0.088 min, or 1.26% of the gradient time. Comparatively, the best commercial quantitative structure-retention relationship model poorly performed, with an <i>R</i>² of 0.11 and mean average error of 0.202 min. This model has been deployed internally as a Dash app to help democratize the use of the developed models and is being used for selecting purification methods based on analyte structure.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144197058","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 Hydrogen Cyanide by Gas Chromatography With Post-Column Reaction and Flame Ionization Detection","authors":"Ronda Gras,&nbsp;Jim Luong,&nbsp;Robert A. Shellie","doi":"10.1002/jssc.70176","DOIUrl":"https://doi.org/10.1002/jssc.70176","url":null,"abstract":"<div>\u0000 \u0000 <p>A straightforward and practical 15-min gas chromatographic method utilizing flame ionization detection has been developed to measure hydrogen cyanide in various matrices. This new approach features a catalyzed two-stage post-column reaction that significantly enhances the detection and quantification of hydrogen cyanide. Selecting the right separation column is crucial for accurate analysis. Initial tests with porous layer open tubular columns resulted in significant peak tailing, rendering them unsuitable for trace-level analysis. Modified polyethylene glycol stationary phases also exhibited strong peak tailing in addition to producing artifact peaks. In contrast, a polydimethylsiloxane-based column with a very low phase ratio (<i>β</i> = 10) demonstrated excellent analytical performance, including peak symmetry and inertness. The analytical approach achieved a minimum detection limit of 50 parts per billion (ppb, v/v) without preconcentration and a linear range from 0.05 to 200 parts per million (ppm, v/v). At a concentration level of 20 ppm (v/v), the RSD at the 95% confidence level was less than 1% (<i>n</i> = 10), and at a concentration level of 1 ppm (v/v), the RSD at the 95% confidence level was less than 3% (<i>n</i> = 10) under the established conditions. The method's effectiveness has been validated through real-life applications, including analyzing hydrogen cyanide in fruit seeds and the headspace of untreated water samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144140470","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":"Effective Separation of Granaticins From Streptomyces Vilmorinianum YP1 Using High-Speed Countercurrent Chromatography and Their Characteristic Evaluation","authors":"Xuechen Si,&nbsp;Huilin Li,&nbsp;Jiarong Yang,&nbsp;Yunping Zhu,&nbsp;Xueli Cao","doi":"10.1002/jssc.70184","DOIUrl":"https://doi.org/10.1002/jssc.70184","url":null,"abstract":"<div>\u0000 \u0000 <p>Granaticins and their derivatives are a series of benzoisochromanequinones (BIQs) compounds with remarkable biological activities, but their practical applications have been restricted due to the low separation efficiency of traditional methods. In this work, a high-speed countercurrent chromatography (HSCCC) method was developed for the first time to separate granaticins from the fermentation broth of <i>Streptomyces vilmorinianum</i> YP1. Considering the similar structures, polarities, and dissociation constants of granaticins, an appropriate solvent system for their complete separation by HSCCC was determined. This system consisted of <i>n</i>-hexane: ethyl acetate: methanol: water in volume ratios of 2: 5: 3: 4 and 1: 4: 1: 4. Five granaticins with high purity were obtained: a granaticin analogue (29.5 mg); granaticin acid (111.3 mg; purity: 99.2%), MM44785 (49.4 mg; purity: 99.1%), granaticin (0.8 mg; purity: 98.7 %), and granaticin B (73.3 mg; purity: 99.4%) from 2.7 g of crude granaticins extract. The antibacterial activity and stability characteristics of the two main compounds were further evaluated. Granaticin B exhibited excellent antibacterial effects on Gram-positive bacteria, while granaticin acid showed better thermal stability. This is the first time to develop a general separation strategy for granaticins that are potentially applicable in industry production.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144140525","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}