Journal of separation science最新文献

{"title":"Rapid and Preparative Separation of Polyphenols From Pods of Paeonia suffruticosa Andr. By Elution-Extrusion Counter-Current Chromatography Coupled With Inner-Recycling Mode","authors":"Xiuheng Qin,&nbsp;Li Xu,&nbsp;Yufa Zhang,&nbsp;Huijiao Yan,&nbsp;Ammara Sohail,&nbsp;Wenshuang Zhao,&nbsp;Daijie Wang,&nbsp;Chao Ma,&nbsp;Li Cui","doi":"10.1002/jssc.70207","DOIUrl":"https://doi.org/10.1002/jssc.70207","url":null,"abstract":"<div>\u0000 \u0000 <p>Pods of <i>Paeonia suffruticosa</i> Andr. are a good source of natural plants and have drawn a lot of interest in order to increase their overall utility value. In this study, elution-extrusion counter-current chromatography coupled with inner-recycling mode was used to successfully extract the polyphenols from <i>Paeonia suffruticosa</i> Andr. pods. Eight compounds, including (1) methyl gallate, (2) 1,2,3,4, 6-trigalloyl-<i>β</i>-<span>d</span>-glucose, (3) methyl digallate (meta- and para- isomers), (4) 4-<i>O</i>-digalloyl-1,2,3,6-tetra-<i>O</i>- galloyl-<i>β</i>-<span>d</span>-glucose, (5) 3-<i>O</i>-digalloyl-1,2,3,6-tetra-<i>O</i>-galloyl-<i>β</i>-<span>d</span>-glucose, (6) (+)-<i>ε</i>-viniferin, (7) amurensin B and (8) gnetin H, were effectively isolated. Structural characterization was performed by nuclear magnetic resonance spectrometry and mass spectrometry. Based on our research, the developed process was a successful way to separate the polyphenols with a broad and similar partition coefficient from pods of <i>Paeonia suffruticosa</i> Andr. It could be used to separate the polyphenols from complicated natural products with the established method.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647175","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":"Flow Injection Inductively Coupled Plasma-Mass Spectrometry With Ultrasonic Nebulizer for the Quantification of Trace Elements in Seawater: An Innovative Method Targeting Cadmium, Cobalt, Lead, Manganese, Molybdenum, Tin, Uranium, and Vanadium","authors":"Giorgia Mattei,&nbsp;Clara Sette,&nbsp;Luca Lucentini,&nbsp;Enrico Veschetti","doi":"10.1002/jssc.70228","DOIUrl":"https://doi.org/10.1002/jssc.70228","url":null,"abstract":"<p>The accurate determination of trace elements in seawater is essential for environmental monitoring and the study of oceanic biogeochemical processes. However, traditional analytical techniques often face limitations due to the ultra-trace concentrations of metals and the high salinity of seawater, which introduces significant matrix effects. In this study, a novel flow injection—inductively coupled plasma mass spectrometry (FI-ICP-MS) method coupled with an ultrasonic nebulizer was developed and optimized for the direct quantification of cadmium, cobalt, lead, manganese, molybdenum, tin, uranium, and vanadium in seawater samples. The method was optimized by evaluating the effects of eluent concentration (0.05–0.20% HNO3, with 0.05% selected as the minimum effective value to ensure analyte stability, prevent precipitation, and minimize salt-related stress on the FI system), flow rate (0.4–1.0 mL/min), and sodium chloride matrix composition, ensuring minimal spectral interferences while maintaining high sensitivity. The selected operating conditions (0.05% HNO3 eluent at 0.70 mL/min with 103Rhodium and 193Iridium as internal standards) provided a robust analytical performance with low procedural limits of detection and quantification (ranging from 0.003 to 0.2 µg/L for LoDs and from 0.01 to 0.7 µg/L for LoQs) and excellent instrumental repeatability (1.2%–6.6%). The overall method was validated using the IAEA-443 seawater certified reference material, yielding recoveries between 104%–118% and procedural reproducibility ranging from 3.8% to 15%.</p><p>The optimized FI-ICP-MS method was applied to real seawater samples collected from two distinct Mediterranean transects: offshore Livorno, a site influenced by intense maritime and industrial activities, and Montecristo Island, a protected marine reserve with minimal anthropogenic impact. Results indicated no significant differences in trace metal concentrations between the two areas, suggesting that natural geochemical processes predominantly regulate elemental distributions. Most elements followed a conservative vertical distribution, with localized anomalies observed for manganese and cadmium. Furthermore, all measured cadmium and lead concentrations were well below the regulatory thresholds set by Directive 2013/39/EU, confirming compliance with environmental quality standards.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70228","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647230","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":"Rapid and Preparative Separation of Polyphenols From Pods of Paeonia suffruticosa Andr. By Elution-Extrusion Counter-Current Chromatography Coupled With Inner-Recycling Mode","authors":"Xiuheng Qin,&nbsp;Li Xu,&nbsp;Yufa Zhang,&nbsp;Huijiao Yan,&nbsp;Ammara Sohail,&nbsp;Wenshuang Zhao,&nbsp;Daijie Wang,&nbsp;Chao Ma,&nbsp;Li Cui","doi":"10.1002/jssc.70207","DOIUrl":"https://doi.org/10.1002/jssc.70207","url":null,"abstract":"<div>\u0000 \u0000 <p>Pods of <i>Paeonia suffruticosa</i> Andr. are a good source of natural plants and have drawn a lot of interest in order to increase their overall utility value. In this study, elution-extrusion counter-current chromatography coupled with inner-recycling mode was used to successfully extract the polyphenols from <i>Paeonia suffruticosa</i> Andr. pods. Eight compounds, including (1) methyl gallate, (2) 1,2,3,4, 6-trigalloyl-<i>β</i>-<span>d</span>-glucose, (3) methyl digallate (meta- and para- isomers), (4) 4-<i>O</i>-digalloyl-1,2,3,6-tetra-<i>O</i>- galloyl-<i>β</i>-<span>d</span>-glucose, (5) 3-<i>O</i>-digalloyl-1,2,3,6-tetra-<i>O</i>-galloyl-<i>β</i>-<span>d</span>-glucose, (6) (+)-<i>ε</i>-viniferin, (7) amurensin B and (8) gnetin H, were effectively isolated. Structural characterization was performed by nuclear magnetic resonance spectrometry and mass spectrometry. Based on our research, the developed process was a successful way to separate the polyphenols with a broad and similar partition coefficient from pods of <i>Paeonia suffruticosa</i> Andr. It could be used to separate the polyphenols from complicated natural products with the established method.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647793","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":"Flow Injection Inductively Coupled Plasma-Mass Spectrometry With Ultrasonic Nebulizer for the Quantification of Trace Elements in Seawater: An Innovative Method Targeting Cadmium, Cobalt, Lead, Manganese, Molybdenum, Tin, Uranium, and Vanadium","authors":"Giorgia Mattei,&nbsp;Clara Sette,&nbsp;Luca Lucentini,&nbsp;Enrico Veschetti","doi":"10.1002/jssc.70228","DOIUrl":"https://doi.org/10.1002/jssc.70228","url":null,"abstract":"<p>The accurate determination of trace elements in seawater is essential for environmental monitoring and the study of oceanic biogeochemical processes. However, traditional analytical techniques often face limitations due to the ultra-trace concentrations of metals and the high salinity of seawater, which introduces significant matrix effects. In this study, a novel flow injection—inductively coupled plasma mass spectrometry (FI-ICP-MS) method coupled with an ultrasonic nebulizer was developed and optimized for the direct quantification of cadmium, cobalt, lead, manganese, molybdenum, tin, uranium, and vanadium in seawater samples. The method was optimized by evaluating the effects of eluent concentration (0.05–0.20% HNO3, with 0.05% selected as the minimum effective value to ensure analyte stability, prevent precipitation, and minimize salt-related stress on the FI system), flow rate (0.4–1.0 mL/min), and sodium chloride matrix composition, ensuring minimal spectral interferences while maintaining high sensitivity. The selected operating conditions (0.05% HNO3 eluent at 0.70 mL/min with 103Rhodium and 193Iridium as internal standards) provided a robust analytical performance with low procedural limits of detection and quantification (ranging from 0.003 to 0.2 µg/L for LoDs and from 0.01 to 0.7 µg/L for LoQs) and excellent instrumental repeatability (1.2%–6.6%). The overall method was validated using the IAEA-443 seawater certified reference material, yielding recoveries between 104%–118% and procedural reproducibility ranging from 3.8% to 15%.</p><p>The optimized FI-ICP-MS method was applied to real seawater samples collected from two distinct Mediterranean transects: offshore Livorno, a site influenced by intense maritime and industrial activities, and Montecristo Island, a protected marine reserve with minimal anthropogenic impact. Results indicated no significant differences in trace metal concentrations between the two areas, suggesting that natural geochemical processes predominantly regulate elemental distributions. Most elements followed a conservative vertical distribution, with localized anomalies observed for manganese and cadmium. Furthermore, all measured cadmium and lead concentrations were well below the regulatory thresholds set by Directive 2013/39/EU, confirming compliance with environmental quality standards.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70228","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647217","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":"Targeted Gas Chromatography-Mass Spectrometry Analysis of 31 Phthalates and Replacements: Method Optimization and Application to Edible Oils and Silicone Wristbands","authors":"Kaley T. Adams,&nbsp;Caoilinn Haggerty,&nbsp;Richard P. Scott,&nbsp;Steven O'Connell,&nbsp;Kim A. Anderson","doi":"10.1002/jssc.70227","DOIUrl":"https://doi.org/10.1002/jssc.70227","url":null,"abstract":"<p>Interest in phthalate detection of foods and other environmental media has grown rapidly in the past decade. However, current analytical and separation techniques are often limited in the breadth of chemistry targeted, most often targeting less than 15 compounds. Challenges to successful methods with this compound group include chromatographic resolution, quantitation across diverse concentration ranges, and sample preparation due to the chemical similarity of these compounds. This project describes the development of a selective ion monitoring gas chromatography mass spectrometry method for quantitation of 29 phthalates and two phthalate replacements along with considerations for quantitation, sample cleanup, and standard storage. Our range of phthalates includes less-studied ones like bis(2-propylheptyl), diundecyl, didecyl, and ditridecyl. Analytical performance included limits of detection ranging from 17–230 ng/mL and robust reproducibility with relative percent differences below 8% for complex matrices. Two calibration ranges were used to accommodate the wide dynamic range of phthalate concentrations observed in real samples. Method application was demonstrated with edible oils (<i>n</i> = 12) and silicone wristbands (<i>n</i> = 18), representing dietary and personal exposure pathways. Sample preparation strategies, including solid phase extraction were evaluated to mitigate matrix interferences. In addition, compound storage stability was assessed over 133 days to inform best practices for standard preparation and handling. The finalized method demonstrates the uniquely large compound ranges for some phthalates and the importance of analyzing a wide variety of these compounds, making it a valuable foundation for comprehensive environmental monitoring of phthalates and their alternatives.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70227","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647473","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":"A Membrane-Based Strategy for the High-Throughput Determination of Steroidal Hormones in Human Urine Using Natural Deep Eutectic Solvents Combined With Liquid Chromatography Coupled With Diode Array Detector","authors":"Lucas Morés,&nbsp;Camila Will,&nbsp;Eduardo Carasek,&nbsp;Josias Merib","doi":"10.1002/jssc.70229","DOIUrl":"https://doi.org/10.1002/jssc.70229","url":null,"abstract":"<p>Estrogen hormones are present in the human body at varying concentrations, either naturally or through ingestion. At regulated levels, these compounds perform vital functions in the body. However, elevated concentrations are related to deregulation of several processes, such as abnormal cell proliferation, which can lead to the development of cancer (breast and ovarian) and other diseases (endometriosis). In this work, an analytical methodology is proposed for the determination of 17β-estradiol (E1), estrone (E2), and 17α-ethinylestradiol (EE2) in human urine. Hollow fiber-microporous membrane liquid–liquid extraction (HF-MMLLE) is used with natural deep eutectic solvents (NADESs). This technique was associated with a 96-well plate system followed by high-performance liquid chromatography coupled with a diode array detector (HPLC-DAD). The optimized conditions consisted of using thymol and camphor (1:1 v/v) as extraction solvent; an extraction time of 100 min; acetonitrile as desorption solvent; a desorption time of 30 min; and a sample pH adjusted to 12. Limits of quantification (LOQs) of 25 ng mL⁻¹ for E2 and 50 ng mL⁻¹ for E1 and EE2, and limits of detection (LOD) of 7.5 ng mL⁻¹ for E2 and 15 ng mL⁻¹ for E1 and EE2 were obtained. Intraday and interday precisions were lower than 8.7% and 21.6%, respectively. Relative recoveries were examined in two samples and ranged from 68.2% to 131.8%. The method was applied in samples from healthy volunteers, and concentrations from 75.6 to 182.7 ng mL⁻¹ for E2 were found. Finally, the method was evaluated by two sustainable metrics to examine the green aspects of the experimental approach.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70229","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647704","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":"Targeted Gas Chromatography-Mass Spectrometry Analysis of 31 Phthalates and Replacements: Method Optimization and Application to Edible Oils and Silicone Wristbands","authors":"Kaley T. Adams,&nbsp;Caoilinn Haggerty,&nbsp;Richard P. Scott,&nbsp;Steven O'Connell,&nbsp;Kim A. Anderson","doi":"10.1002/jssc.70227","DOIUrl":"https://doi.org/10.1002/jssc.70227","url":null,"abstract":"<p>Interest in phthalate detection of foods and other environmental media has grown rapidly in the past decade. However, current analytical and separation techniques are often limited in the breadth of chemistry targeted, most often targeting less than 15 compounds. Challenges to successful methods with this compound group include chromatographic resolution, quantitation across diverse concentration ranges, and sample preparation due to the chemical similarity of these compounds. This project describes the development of a selective ion monitoring gas chromatography mass spectrometry method for quantitation of 29 phthalates and two phthalate replacements along with considerations for quantitation, sample cleanup, and standard storage. Our range of phthalates includes less-studied ones like bis(2-propylheptyl), diundecyl, didecyl, and ditridecyl. Analytical performance included limits of detection ranging from 17–230 ng/mL and robust reproducibility with relative percent differences below 8% for complex matrices. Two calibration ranges were used to accommodate the wide dynamic range of phthalate concentrations observed in real samples. Method application was demonstrated with edible oils (<i>n</i> = 12) and silicone wristbands (<i>n</i> = 18), representing dietary and personal exposure pathways. Sample preparation strategies, including solid phase extraction were evaluated to mitigate matrix interferences. In addition, compound storage stability was assessed over 133 days to inform best practices for standard preparation and handling. The finalized method demonstrates the uniquely large compound ranges for some phthalates and the importance of analyzing a wide variety of these compounds, making it a valuable foundation for comprehensive environmental monitoring of phthalates and their alternatives.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70227","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647298","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":"Integrating LC-MS/MS and Molecular Networking for Advance Analysis and Comprehensive Flavonoids Annotation","authors":"Priscillia Ann David,&nbsp;Anis Irfan Norazhar,&nbsp;Mohamad Shazeli Che Zain","doi":"10.1002/jssc.70230","DOIUrl":"https://doi.org/10.1002/jssc.70230","url":null,"abstract":"<div>\u0000 \u0000 <p>Flavonoids, a subclass of phenolic compounds, exhibit diverse therapeutic properties, including antioxidant, anti-inflammatory, and wound healing properties. These health-promoting effects of flavonoids are greatly dependent on the variation in their structural diversity, which are generally perceived as complex metabolomic datasets. Among detection techniques used, state-of-the-art high-resolution liquid chromatography hyphenated with tandem mass spectrometry (LC-MS/MS) has become a popular analytical method of choice for the analysis of flavonoids from various plant tissue extracts. Despite its broad applicability, the vast amount and complexity of fragmentation data produced have made the comprehensive identification of flavonoids remains a key challenge. An offshoot of metabolomics, currently, molecular networking (MN), a computational approach based on MS/MS data, has emerged as a revolutionary technique for identifying and characterizing numerous flavonoid molecular families. By visualizing the spectral similarities of flavonoid fingerprints, MN enables rapid dereplication, efficient in assisting annotation of unknown features with known chemical scaffolds, and demonstrates high precision in resolving structurally diverse flavonoid isomers. Various MN tools, i.e., classical molecular networking (CLMN), feature-based molecular networking (FBMN), and substructure-based MN (MS2LDA), streamline the identification process and improve the understanding of flavonoids biosynthesis. This review aimed to describe the recent advancement in MS-based strategy for flavonoids characterization, starting with an overview on the application of LC-MS/MS and its limitation in the typical dereplication workflow, followed by specific sections on MN techniques, highlighting the aspects of general principles, workflow, and its application in flavonoid research.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647475","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":"Integrating LC-MS/MS and Molecular Networking for Advance Analysis and Comprehensive Flavonoids Annotation","authors":"Priscillia Ann David,&nbsp;Anis Irfan Norazhar,&nbsp;Mohamad Shazeli Che Zain","doi":"10.1002/jssc.70230","DOIUrl":"https://doi.org/10.1002/jssc.70230","url":null,"abstract":"<div>\u0000 \u0000 <p>Flavonoids, a subclass of phenolic compounds, exhibit diverse therapeutic properties, including antioxidant, anti-inflammatory, and wound healing properties. These health-promoting effects of flavonoids are greatly dependent on the variation in their structural diversity, which are generally perceived as complex metabolomic datasets. Among detection techniques used, state-of-the-art high-resolution liquid chromatography hyphenated with tandem mass spectrometry (LC-MS/MS) has become a popular analytical method of choice for the analysis of flavonoids from various plant tissue extracts. Despite its broad applicability, the vast amount and complexity of fragmentation data produced have made the comprehensive identification of flavonoids remains a key challenge. An offshoot of metabolomics, currently, molecular networking (MN), a computational approach based on MS/MS data, has emerged as a revolutionary technique for identifying and characterizing numerous flavonoid molecular families. By visualizing the spectral similarities of flavonoid fingerprints, MN enables rapid dereplication, efficient in assisting annotation of unknown features with known chemical scaffolds, and demonstrates high precision in resolving structurally diverse flavonoid isomers. Various MN tools, i.e., classical molecular networking (CLMN), feature-based molecular networking (FBMN), and substructure-based MN (MS2LDA), streamline the identification process and improve the understanding of flavonoids biosynthesis. This review aimed to describe the recent advancement in MS-based strategy for flavonoids characterization, starting with an overview on the application of LC-MS/MS and its limitation in the typical dereplication workflow, followed by specific sections on MN techniques, highlighting the aspects of general principles, workflow, and its application in flavonoid research.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647705","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":"A Membrane-Based Strategy for the High-Throughput Determination of Steroidal Hormones in Human Urine Using Natural Deep Eutectic Solvents Combined With Liquid Chromatography Coupled With Diode Array Detector","authors":"Lucas Morés,&nbsp;Camila Will,&nbsp;Eduardo Carasek,&nbsp;Josias Merib","doi":"10.1002/jssc.70229","DOIUrl":"https://doi.org/10.1002/jssc.70229","url":null,"abstract":"<p>Estrogen hormones are present in the human body at varying concentrations, either naturally or through ingestion. At regulated levels, these compounds perform vital functions in the body. However, elevated concentrations are related to deregulation of several processes, such as abnormal cell proliferation, which can lead to the development of cancer (breast and ovarian) and other diseases (endometriosis). In this work, an analytical methodology is proposed for the determination of 17β-estradiol (E1), estrone (E2), and 17α-ethinylestradiol (EE2) in human urine. Hollow fiber-microporous membrane liquid–liquid extraction (HF-MMLLE) is used with natural deep eutectic solvents (NADESs). This technique was associated with a 96-well plate system followed by high-performance liquid chromatography coupled with a diode array detector (HPLC-DAD). The optimized conditions consisted of using thymol and camphor (1:1 v/v) as extraction solvent; an extraction time of 100 min; acetonitrile as desorption solvent; a desorption time of 30 min; and a sample pH adjusted to 12. Limits of quantification (LOQs) of 25 ng mL⁻¹ for E2 and 50 ng mL⁻¹ for E1 and EE2, and limits of detection (LOD) of 7.5 ng mL⁻¹ for E2 and 15 ng mL⁻¹ for E1 and EE2 were obtained. Intraday and interday precisions were lower than 8.7% and 21.6%, respectively. Relative recoveries were examined in two samples and ranged from 68.2% to 131.8%. The method was applied in samples from healthy volunteers, and concentrations from 75.6 to 182.7 ng mL⁻¹ for E2 were found. Finally, the method was evaluated by two sustainable metrics to examine the green aspects of the experimental approach.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70229","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647474","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}