An environmental friendly, fast, easy and inexpensive pH-switchable hydrophobic deep eutectic solvent-based liquid phase microextraction procedure was developed and combined with HPLC-UV detection for the extraction and analysis of morphine and codeine in whole blood samples. In this method, seven deep eutectic solvents were synthesized and then their switchability with pH was investigated. Deep eutectic solvents that could be switched with pH were used as extractant. Under the optimum conditions, relative standard deviation values for intra-day and inter-day of the method based on seven replicate measurements of 50 μg L-1 of morphine and codeine in blood samples were in the range of 3.7-4.3% and 5.4-6.2%, respectively. The calibration graphs were linear in the range of 1.5-300 μg L-1 and limit of detection for both analytes was 0.5 μg L-1. The enrichment factor and the extraction recovery of morphine and codeine were in the ranges of 152-166, and 76-83%, respectively. The results showed that both morphine and codeine were detected in the blood sample of the addicted person. The relative recoveries of real blood samples which have been spiked with different levels of morphine and codeine were 91.8-107.0%. This article is protected by copyright. All rights reserved.
{"title":"Trace determination of morphine and codeine in whole blood samples using pH-switchable hydrophobic deep eutectic solvents based liquid phase microextraction followed by HPLC-UV.","authors":"Fuad Ameen","doi":"10.1002/jssc.202300336","DOIUrl":"https://doi.org/10.1002/jssc.202300336","url":null,"abstract":"<p><p>An environmental friendly, fast, easy and inexpensive pH-switchable hydrophobic deep eutectic solvent-based liquid phase microextraction procedure was developed and combined with HPLC-UV detection for the extraction and analysis of morphine and codeine in whole blood samples. In this method, seven deep eutectic solvents were synthesized and then their switchability with pH was investigated. Deep eutectic solvents that could be switched with pH were used as extractant. Under the optimum conditions, relative standard deviation values for intra-day and inter-day of the method based on seven replicate measurements of 50 μg L<sup>-1</sup> of morphine and codeine in blood samples were in the range of 3.7-4.3% and 5.4-6.2%, respectively. The calibration graphs were linear in the range of 1.5-300 μg L<sup>-1</sup> and limit of detection for both analytes was 0.5 μg L<sup>-1</sup>. The enrichment factor and the extraction recovery of morphine and codeine were in the ranges of 152-166, and 76-83%, respectively. The results showed that both morphine and codeine were detected in the blood sample of the addicted person. The relative recoveries of real blood samples which have been spiked with different levels of morphine and codeine were 91.8-107.0%. This article is protected by copyright. All rights reserved.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":" ","pages":"e2300336"},"PeriodicalIF":2.8,"publicationDate":"2025-12-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145743166","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}
Nathalie Le Bris, Axel Beringue, Johanna Rivas, David Renault, Marion Chorin, Hervé Colinet
The technical progress of metabolomics—the analysis of metabolite composition of cells, tissues, and biofluids—and its ability to unravel phenotypical responses of organisms to their environment was accompanied by the democratization of their use in a wide range of scientific fields. While the reliability of analytical procedures was thoroughly assessed, the effects of preanalytical processing on sample metabolic profiles (i.e., conditioning, storage, transportation, etc.) remain quite unclear. This uncertainty is especially notable for samples collected in the frame of ecological studies, which often involve field sampling and remote sample production, leading to extended transportation durations and suboptimal storage conditions. In this study, we evaluated the impact of storage duration and temperature, along with the effects of freeze-drying (or lyophilization; the process of stabilization through dehydration by sublimation), on the metabolic profiles of samples relevant to ecological studies. Specifically, we focused on the lesser mealworm (Alphitobius diaperinus), the fruit fly (Drosophila melanogaster), and the perennial ryegrass (Lolium perenne). The levels of 60 different metabolites were quantitatively analyzed using targeted metabolomics through gas chromatography–mass spectrometry (GC–MS). We report significant metabolic shifts associated with freeze-drying, resulting in both increases and decreases in the contents of more than half of the quantified metabolites across all assessed chemical families. Several amino acids exhibited more than a fourfold increase in all investigated matrices. Furthermore, while samples stored at −80°C exhibited profiles most similar to those of samples analyzed right after collection, the metabolic profiles of these samples gradually changed over the 6 months of storage. Interestingly, metabolic shifts related to sample preanalytical processing and storage were relatively consistent across the biological matrices studied, particularly between the two insect species. Based on these observations, we propose several recommendations for reliable preanalytical sample processing in ecological studies, considering logistical and economic constraints.
{"title":"How to Process Samples for Metabolomics in Ecology: A Comparative Study of Preanalytical Storage Methods","authors":"Nathalie Le Bris, Axel Beringue, Johanna Rivas, David Renault, Marion Chorin, Hervé Colinet","doi":"10.1002/jssc.70333","DOIUrl":"10.1002/jssc.70333","url":null,"abstract":"<p>The technical progress of metabolomics—the analysis of metabolite composition of cells, tissues, and biofluids—and its ability to unravel phenotypical responses of organisms to their environment was accompanied by the democratization of their use in a wide range of scientific fields. While the reliability of analytical procedures was thoroughly assessed, the effects of preanalytical processing on sample metabolic profiles (i.e., conditioning, storage, transportation, etc.) remain quite unclear. This uncertainty is especially notable for samples collected in the frame of ecological studies, which often involve field sampling and remote sample production, leading to extended transportation durations and suboptimal storage conditions. In this study, we evaluated the impact of storage duration and temperature, along with the effects of freeze-drying (or lyophilization; the process of stabilization through dehydration by sublimation), on the metabolic profiles of samples relevant to ecological studies. Specifically, we focused on the lesser mealworm (<i>Alphitobius diaperinus</i>), the fruit fly (<i>Drosophila melanogaster</i>), and the perennial ryegrass (<i>Lolium perenne</i>). The levels of 60 different metabolites were quantitatively analyzed using targeted metabolomics through gas chromatography–mass spectrometry (GC–MS). We report significant metabolic shifts associated with freeze-drying, resulting in both increases and decreases in the contents of more than half of the quantified metabolites across all assessed chemical families. Several amino acids exhibited more than a fourfold increase in all investigated matrices. Furthermore, while samples stored at −80°C exhibited profiles most similar to those of samples analyzed right after collection, the metabolic profiles of these samples gradually changed over the 6 months of storage. Interestingly, metabolic shifts related to sample preanalytical processing and storage were relatively consistent across the biological matrices studied, particularly between the two insect species. Based on these observations, we propose several recommendations for reliable preanalytical sample processing in ecological studies, considering logistical and economic constraints.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12690189/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145714502","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}
Obtaining an insight into the composition of fuel and process intermediates samples is important for monitoring of the product quality, production and exploitation process improvement and complying with industry and environmental regulations. A broadband vacuum ultraviolet (VUV) spectroscopy detector has been successfully hyphenated with both GC and comprehensive two-dimensional gas chromatography (GC×GC) for the analysis of various fuel samples. This detector possesses both qualitative and quantitative capabilities. Most compounds absorb in the vacuum ultraviolet spectral range, and they exhibit rich and distinctive spectral features. Main constituents of fuel samples, hydrocarbons, such as paraffins, olefins, naphthenes, aromatics are identified with the VUV with very good selectivity. As data obtained from the GC×GC-VUV analysis of fuels can be challenging to exploit due to the sample complexity, it can be useful to employ chemometric methods for fuel composition exploration in a fast and efficient manner. In this work, 14 gas oil samples were analysed by GC×GC-VUV and after suitable data preprocessing, a pixel-based approach combined with k-means clustering was applied in order to classify compounds’ spectra into major hydrocarbon families in each sample and obtain a semi-quantification result which was then compared with the results of mass spectrometry analysis and quantitative GC×GC-VUV that involved application of detailed identification templates and response factors. It was demonstrated that due to hydrocarbon families exhibiting similar VUV absorbance spectra, the proposed workflow for GC×GC-VUV data preprocessing and analysis can be a fast and efficient way for gas oils global composition exploration.
{"title":"Spectral Pixel-Based Analysis and Clustering Workflow for the Exploration of the Composition of Gas Oil Samples by Comprehensive Two-dimensional Gas Chromatography Vacuum Ultraviolet Spectroscopy","authors":"Aleksandra Lelevic","doi":"10.1002/jssc.70318","DOIUrl":"10.1002/jssc.70318","url":null,"abstract":"<p>Obtaining an insight into the composition of fuel and process intermediates samples is important for monitoring of the product quality, production and exploitation process improvement and complying with industry and environmental regulations. A broadband vacuum ultraviolet (VUV) spectroscopy detector has been successfully hyphenated with both GC and comprehensive two-dimensional gas chromatography (GC×GC) for the analysis of various fuel samples. This detector possesses both qualitative and quantitative capabilities. Most compounds absorb in the vacuum ultraviolet spectral range, and they exhibit rich and distinctive spectral features. Main constituents of fuel samples, hydrocarbons, such as paraffins, olefins, naphthenes, aromatics are identified with the VUV with very good selectivity. As data obtained from the GC×GC-VUV analysis of fuels can be challenging to exploit due to the sample complexity, it can be useful to employ chemometric methods for fuel composition exploration in a fast and efficient manner. In this work, 14 gas oil samples were analysed by GC×GC-VUV and after suitable data preprocessing, a pixel-based approach combined with k-means clustering was applied in order to classify compounds’ spectra into major hydrocarbon families in each sample and obtain a semi-quantification result which was then compared with the results of mass spectrometry analysis and quantitative GC×GC-VUV that involved application of detailed identification templates and response factors. It was demonstrated that due to hydrocarbon families exhibiting similar VUV absorbance spectra, the proposed workflow for GC×GC-VUV data preprocessing and analysis can be a fast and efficient way for gas oils global composition exploration.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12683198/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145701235","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}
Naiding Wang, Jun Zhang, Yanqing Duan, Ruizhi Zhu, Lei Yang, Juxing Jiang, Hongkun Li, Yanqun Xu, Zhigang Tai
Plant-derived squalene represents a vital natural source of high additional value product, yet conventional extraction methods are often hindered by their reliance on large volumes of organic solvents, limiting their widespread application. Here, we developed a pioneering green extraction platform integrating ultrasonic-assisted extraction with ternary deep eutectic solvents (UAE–TDESs), specifically engineered for efficient squalene recovery from plant biomass. Through systematic optimization via response surface methodology (RSM), we achieved a maximum squalene yield of 331.79 µg/g dry weight (DW) under optimal conditions: TDESs (betaine: vitamin C: glycerol, 2:1:1 molar ratio), 69°C extraction temperature, 41 min duration, 31 mL/g liquid–solid ratio, and 39% TDES water content. Comparative analysis demonstrated a 2.9% yield enhancement over the n-hexane extraction (322.58 µg/g DW) while eliminating all toxic organic solvents. Mechanistic investigations using scanning electron microscopy (SEM) and x-ray diffraction (XRD) revealed that TDESs induce lignin dissolution while ultrasonication disrupted cellular architecture through cavitation-driven mechanical shear. Collectively, this work established a robust, sustainable framework for TDESs mediated recovery of bioactive compounds, demonstrating significant potential for broader industrial application.
{"title":"Ultrasound-Assisted Combined With Natural Ternary Deep Eutectic Solvent Extraction Method for the Green Extraction of Squalene From Strobilanthes tonkinensis","authors":"Naiding Wang, Jun Zhang, Yanqing Duan, Ruizhi Zhu, Lei Yang, Juxing Jiang, Hongkun Li, Yanqun Xu, Zhigang Tai","doi":"10.1002/jssc.70332","DOIUrl":"10.1002/jssc.70332","url":null,"abstract":"<div>\u0000 \u0000 <p>Plant-derived squalene represents a vital natural source of high additional value product, yet conventional extraction methods are often hindered by their reliance on large volumes of organic solvents, limiting their widespread application. Here, we developed a pioneering green extraction platform integrating ultrasonic-assisted extraction with ternary deep eutectic solvents (UAE–TDESs), specifically engineered for efficient squalene recovery from plant biomass. Through systematic optimization via response surface methodology (RSM), we achieved a maximum squalene yield of 331.79 µg/g dry weight (DW) under optimal conditions: TDESs (betaine: vitamin C: glycerol, 2:1:1 molar ratio), 69°C extraction temperature, 41 min duration, 31 mL/g liquid–solid ratio, and 39% TDES water content. Comparative analysis demonstrated a 2.9% yield enhancement over the <i>n</i>-hexane extraction (322.58 µg/g DW) while eliminating all toxic organic solvents. Mechanistic investigations using scanning electron microscopy (SEM) and x-ray diffraction (XRD) revealed that TDESs induce lignin dissolution while ultrasonication disrupted cellular architecture through cavitation-driven mechanical shear. Collectively, this work established a robust, sustainable framework for TDESs mediated recovery of bioactive compounds, demonstrating significant potential for broader industrial application.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145701233","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}
Monoclonal antibodies are biopharmaceuticals used to treat various diseases, including autoimmune disorders and cancer. Due to their structural complexity and inherent heterogeneity, robust analytical methods are required for their accurate quantification and quality control. This study presents a novel middle-up (MU) capillary zone electrophoresis-mass spectrometry (CZE-MS) method for the quantitative analysis of infliximab (IFX), a widely used therapeutic mAb. The method relies on disulfide bond reduction to separate heavy and light chains, followed by CZE separation using a 2 M acetic acid background electrolyte and MS detection in single ion monitoring mode. Adalimumab was used as an internal standard, providing a suitable alternative to isotopically labeled monoclonal antibody analogues. Evaluation of the analytical method performance followed ICH Q2(R1) guidelines and demonstrated an acceptable linearity range (4–35 µg/mL), precision, accuracy, and a limit of quantification of 4 µg/mL. The method was successfully applied to quantify IFX in a commercial pharmaceutical (Remicade). Moreover, the method was preliminarily tested for the quality control of bevacizumab in Avastin and rituximab in MabThera pharmaceutical formulations. To our knowledge, this is the first report of quantitative MU CZE-MS analysis of therapeutic monoclonal antibodies directly from pharmaceutical matrices, highlighting its potential for quality drug control applications.
{"title":"Quantification of Monoclonal Antibodies in Pharmaceutical Matrices by Middle-Up Capillary Zone Electrophoresis-Mass Spectrometry","authors":"Jana Havlikova, Katarina Marakova, Peter Mikus","doi":"10.1002/jssc.70335","DOIUrl":"10.1002/jssc.70335","url":null,"abstract":"<div>\u0000 \u0000 <p>Monoclonal antibodies are biopharmaceuticals used to treat various diseases, including autoimmune disorders and cancer. Due to their structural complexity and inherent heterogeneity, robust analytical methods are required for their accurate quantification and quality control. This study presents a novel middle-up (MU) capillary zone electrophoresis-mass spectrometry (CZE-MS) method for the quantitative analysis of infliximab (IFX), a widely used therapeutic mAb. The method relies on disulfide bond reduction to separate heavy and light chains, followed by CZE separation using a 2 M acetic acid background electrolyte and MS detection in single ion monitoring mode. Adalimumab was used as an internal standard, providing a suitable alternative to isotopically labeled monoclonal antibody analogues. Evaluation of the analytical method performance followed ICH Q2(R1) guidelines and demonstrated an acceptable linearity range (4–35 µg/mL), precision, accuracy, and a limit of quantification of 4 µg/mL. The method was successfully applied to quantify IFX in a commercial pharmaceutical (Remicade). Moreover, the method was preliminarily tested for the quality control of bevacizumab in Avastin and rituximab in MabThera pharmaceutical formulations. To our knowledge, this is the first report of quantitative MU CZE-MS analysis of therapeutic monoclonal antibodies directly from pharmaceutical matrices, highlighting its potential for quality drug control applications.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145701100","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}
Acanthopanax senticosus (AS) is a well-known traditional herbal medicine in China that can invigorate the spleen, tonify the qi and kidney, tranquilize the mind, and possess diverse bioactive functions. However, comprehensive and simultaneous analysis of the main active constituents from AS and in vivo metabolites remains underexplored, which severely impedes its further clinical application. In this study, AB-8 macroporous resin column chromatography was used to enrich the AS extract. Furthermore, ultrahigh performance liquid chromatography with quadrupole time of flight mass spectrometry (UHPLC–Q-TOF-MS/MS) and UPLC-Q-Orbitrap MS techniques were utilized to identify and characterize the chemical constituents and in vivo metabolites of AS extract, respectively. As a result, a total of 60 components were characterized in the AS extract, including 33 phenylpropanoids, 13 lignans, 4 coumarins, and 10 other substances. Additionally, a total of 29 prototype components and 226 metabolites were detected. Specifically, 91 metabolites were discovered in plasma, 19 in brain tissue, 111 in urine, and 76 in feces. The metabolic reactions included Phase I reactions (demethylation, deglucose, oxidation, and hydration) and Phase II reactions (methylation, sulfate esterification, glucuronidation, glucose conjugation, glycine conjugation, and acetylation). In conclusion, our findings provided basic data and a method for further investigations into the relationship between the chemical composition and pharmacological effects of AS. These results are valuable for revealing the material basis, illustrating the mechanism of medical action, and guiding the clinical applications of AS.
{"title":"Comprehensive Characterization of the Chemical Constituents, Absorbed Prototypes, and Metabolic Profiles of Acanthopanax senticosus Extract Based on Ultrahigh-Performance Liquid Chromatography–Mass Spectrometry","authors":"Jing Wang, Ying Li, Jingyi Yu, Rong Shi, Cheng Zhao, Ting Zhang, Mingmei Zhou","doi":"10.1002/jssc.70327","DOIUrl":"https://doi.org/10.1002/jssc.70327","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Acanthopanax senticosus</i> (AS) is a well-known traditional herbal medicine in China that can invigorate the spleen, tonify the qi and kidney, tranquilize the mind, and possess diverse bioactive functions. However, comprehensive and simultaneous analysis of the main active constituents from AS and in vivo metabolites remains underexplored, which severely impedes its further clinical application. In this study, AB-8 macroporous resin column chromatography was used to enrich the AS extract. Furthermore, ultrahigh performance liquid chromatography with quadrupole time of flight mass spectrometry (UHPLC–Q-TOF-MS/MS) and UPLC-Q-Orbitrap MS techniques were utilized to identify and characterize the chemical constituents and in vivo metabolites of AS extract, respectively. As a result, a total of 60 components were characterized in the AS extract, including 33 phenylpropanoids, 13 lignans, 4 coumarins, and 10 other substances. Additionally, a total of 29 prototype components and 226 metabolites were detected. Specifically, 91 metabolites were discovered in plasma, 19 in brain tissue, 111 in urine, and 76 in feces. The metabolic reactions included Phase I reactions (demethylation, deglucose, oxidation, and hydration) and Phase II reactions (methylation, sulfate esterification, glucuronidation, glucose conjugation, glycine conjugation, and acetylation). In conclusion, our findings provided basic data and a method for further investigations into the relationship between the chemical composition and pharmacological effects of AS. These results are valuable for revealing the material basis, illustrating the mechanism of medical action, and guiding the clinical applications of AS.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-11-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145619306","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}
Acanthopanax senticosus (AS) is a well-known traditional herbal medicine in China that can invigorate the spleen, tonify the qi and kidney, tranquilize the mind, and possess diverse bioactive functions. However, comprehensive and simultaneous analysis of the main active constituents from AS and in vivo metabolites remains underexplored, which severely impedes its further clinical application. In this study, AB-8 macroporous resin column chromatography was used to enrich the AS extract. Furthermore, ultrahigh performance liquid chromatography with quadrupole time of flight mass spectrometry (UHPLC–Q-TOF-MS/MS) and UPLC-Q-Orbitrap MS techniques were utilized to identify and characterize the chemical constituents and in vivo metabolites of AS extract, respectively. As a result, a total of 60 components were characterized in the AS extract, including 33 phenylpropanoids, 13 lignans, 4 coumarins, and 10 other substances. Additionally, a total of 29 prototype components and 226 metabolites were detected. Specifically, 91 metabolites were discovered in plasma, 19 in brain tissue, 111 in urine, and 76 in feces. The metabolic reactions included Phase I reactions (demethylation, deglucose, oxidation, and hydration) and Phase II reactions (methylation, sulfate esterification, glucuronidation, glucose conjugation, glycine conjugation, and acetylation). In conclusion, our findings provided basic data and a method for further investigations into the relationship between the chemical composition and pharmacological effects of AS. These results are valuable for revealing the material basis, illustrating the mechanism of medical action, and guiding the clinical applications of AS.
{"title":"Comprehensive Characterization of the Chemical Constituents, Absorbed Prototypes, and Metabolic Profiles of Acanthopanax senticosus Extract Based on Ultrahigh-Performance Liquid Chromatography–Mass Spectrometry","authors":"Jing Wang, Ying Li, Jingyi Yu, Rong Shi, Cheng Zhao, Ting Zhang, Mingmei Zhou","doi":"10.1002/jssc.70327","DOIUrl":"https://doi.org/10.1002/jssc.70327","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Acanthopanax senticosus</i> (AS) is a well-known traditional herbal medicine in China that can invigorate the spleen, tonify the qi and kidney, tranquilize the mind, and possess diverse bioactive functions. However, comprehensive and simultaneous analysis of the main active constituents from AS and in vivo metabolites remains underexplored, which severely impedes its further clinical application. In this study, AB-8 macroporous resin column chromatography was used to enrich the AS extract. Furthermore, ultrahigh performance liquid chromatography with quadrupole time of flight mass spectrometry (UHPLC–Q-TOF-MS/MS) and UPLC-Q-Orbitrap MS techniques were utilized to identify and characterize the chemical constituents and in vivo metabolites of AS extract, respectively. As a result, a total of 60 components were characterized in the AS extract, including 33 phenylpropanoids, 13 lignans, 4 coumarins, and 10 other substances. Additionally, a total of 29 prototype components and 226 metabolites were detected. Specifically, 91 metabolites were discovered in plasma, 19 in brain tissue, 111 in urine, and 76 in feces. The metabolic reactions included Phase I reactions (demethylation, deglucose, oxidation, and hydration) and Phase II reactions (methylation, sulfate esterification, glucuronidation, glucose conjugation, glycine conjugation, and acetylation). In conclusion, our findings provided basic data and a method for further investigations into the relationship between the chemical composition and pharmacological effects of AS. These results are valuable for revealing the material basis, illustrating the mechanism of medical action, and guiding the clinical applications of AS.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-11-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145619320","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}
Mila Č. Lazović, Mihajlo V. Jakanovski, Sandra B. Šegan, Dušanka M. Milojković-Opsenica, Mirjana D. Mosić
Phenolic compounds, secondary metabolites, are essential products of plant metabolism. They are characterized by one or more aromatic rings attached to hydroxyl groups and are categorized into phenolic acids, flavonoids, tannins, stilbenes, and lignans. These compounds play critical roles in plants, contributing to pigmentation, astringency, UV protection, and defense against pests and pathogens. Widely distributed in fruits, vegetables, and other matrices, they are also extracted from waste and byproducts of the food production chain, aligning with sustainable practices. Research on phenolic compounds is extensive, driven by their significant health benefits and diverse biological activity. Extraction is the initial and critical step in their study, with efficiency influenced by factors such as the extraction method, plant matrix properties, solvent choice, temperature, pressure, and time. Recent years have seen a surge in studies on both conventional and innovative extraction methodologies, with a growing emphasis on green technologies. This review provides a comprehensive overview of advancements in green sample preparation (GSP) techniques within the framework of green analytical chemistry (GAC). It highlights strategies to minimize environmental impact, including the use of micro-techniques, assisted extraction methods, and eco-friendly solvents from renewable and non-toxic sources. Experimental design methods for optimizing phenolic compound yields are also discussed. Additionally, the review presents tools for assessing the greenness of sample preparation techniques, focusing on their environmental and operational improvements.
{"title":"Recent Progress in Green Sample Preparation for Improved Plant-Based Natural Product and Phenolic Compound Analysis","authors":"Mila Č. Lazović, Mihajlo V. Jakanovski, Sandra B. Šegan, Dušanka M. Milojković-Opsenica, Mirjana D. Mosić","doi":"10.1002/jssc.70325","DOIUrl":"https://doi.org/10.1002/jssc.70325","url":null,"abstract":"<div>\u0000 \u0000 <p>Phenolic compounds, secondary metabolites, are essential products of plant metabolism. They are characterized by one or more aromatic rings attached to hydroxyl groups and are categorized into phenolic acids, flavonoids, tannins, stilbenes, and lignans. These compounds play critical roles in plants, contributing to pigmentation, astringency, UV protection, and defense against pests and pathogens. Widely distributed in fruits, vegetables, and other matrices, they are also extracted from waste and byproducts of the food production chain, aligning with sustainable practices. Research on phenolic compounds is extensive, driven by their significant health benefits and diverse biological activity. Extraction is the initial and critical step in their study, with efficiency influenced by factors such as the extraction method, plant matrix properties, solvent choice, temperature, pressure, and time. Recent years have seen a surge in studies on both conventional and innovative extraction methodologies, with a growing emphasis on green technologies. This review provides a comprehensive overview of advancements in green sample preparation (GSP) techniques within the framework of green analytical chemistry (GAC). It highlights strategies to minimize environmental impact, including the use of micro-techniques, assisted extraction methods, and eco-friendly solvents from renewable and non-toxic sources. Experimental design methods for optimizing phenolic compound yields are also discussed. Additionally, the review presents tools for assessing the greenness of sample preparation techniques, focusing on their environmental and operational improvements.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-11-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145619254","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}
Wenmin Zhang, Baodi Liao, Jinyu Zhang, Min Fang, Lan Zhang
Okadaic acid is a fatty acid polyether biotoxin that poses a significant threat to global human health. In this work, a type of heterogeneous microporous organic network films was synthesized using a surface-initiated polymerization method, which was employed to control the growth of microporous organic network onto the bromine-functionalized surface of a polymer film. The resulting microporous organic network films feature a porous structure, a strong hydrophobic surface, excellent chemical stability, a large specific surface area, and abundant adsorption sites. These films were then applied in film-based solid-phase extraction, and showed outstanding extraction performance for okadaic acid. Under optimized conditions, the film-based solid-phase extraction method was combined with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) to establish a new analytical method with high sensitivity and efficiency. The developed method offers a wide linear range (2.0–1000.0 pg mL−1) with good linearity (r ≥ 0.9998), a low detection limit (0.5 pg mL−1), and high precision (RSDs ≤ 5.2%, n = 5). This method was further utilized for the determination of okadaic acid in seafood, successfully detecting trace levels of okadaic acid (5.4 and 13.9 pg mL−1) with satisfactory recoveries (85.4%–105.8%). The results indicate that the microporous organic network films hold great application potential in sample pretreatment, and provide a novel synthesis strategy for microporous organic network films.
{"title":"A Surface-Initiated Polymerized Microporous Organic Network Film for Efficient Extraction of Okadaic Acid From Seafood","authors":"Wenmin Zhang, Baodi Liao, Jinyu Zhang, Min Fang, Lan Zhang","doi":"10.1002/jssc.70330","DOIUrl":"10.1002/jssc.70330","url":null,"abstract":"<div>\u0000 \u0000 <p>Okadaic acid is a fatty acid polyether biotoxin that poses a significant threat to global human health. In this work, a type of heterogeneous microporous organic network films was synthesized using a surface-initiated polymerization method, which was employed to control the growth of microporous organic network onto the bromine-functionalized surface of a polymer film. The resulting microporous organic network films feature a porous structure, a strong hydrophobic surface, excellent chemical stability, a large specific surface area, and abundant adsorption sites. These films were then applied in film-based solid-phase extraction, and showed outstanding extraction performance for okadaic acid. Under optimized conditions, the film-based solid-phase extraction method was combined with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) to establish a new analytical method with high sensitivity and efficiency. The developed method offers a wide linear range (2.0–1000.0 pg mL<sup>−1</sup>) with good linearity (<i>r</i> ≥ 0.9998), a low detection limit (0.5 pg mL<sup>−1</sup>), and high precision (RSDs ≤ 5.2%, <i>n</i> = 5). This method was further utilized for the determination of okadaic acid in seafood, successfully detecting trace levels of okadaic acid (5.4 and 13.9 pg mL<sup>−1</sup>) with satisfactory recoveries (85.4%–105.8%). The results indicate that the microporous organic network films hold great application potential in sample pretreatment, and provide a novel synthesis strategy for microporous organic network films.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-11-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145619248","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}
Kai Zhong, Yingjian Guo, Yuning Wang, Longsheng Guo, Lei Zhao, Tao Yue, Hui Wang, Jinqian Yu
A novel strategy combining XAD-4 macroporous resin pretreatment and online-storage inner-recycling high-speed counter-current chromatography (OS-IRCCC) was developed for efficient separation of multi-polarity constituents from Polygonatum cyrtonema Hua. The innovation lies in the OS-IRCCC mode, which integrates online storage of target fractions via a six-way valve-equipped recycling loop and inner-recycling separation, overcoming limitations of conventional high-speed counter-current chromatography in resolving structurally similar compounds. After resin fractionation, 40%, 60%, and 95% ethanol eluates were separated using methyl tert-butyl ether/n-butanol/acetonitrile/water (1:4:1:5, v/v) solvent system, chloroform/methanol/water (7:6:4, v/v) solvent system (with OS-IRCCC for Compounds 8 and 9), and petroleum ether/ethyl acetate/methanol/water (5:5:4:3, v/v) solvent system, respectively. Thirteen compounds were successfully isolated, including four high-polarity glycosides (1–4), five medium-polarity phenolic constituents (5–9), and four low-polarity terpenes (10–13). This study demonstrates that the established separation method provides an efficient, rapid, and straightforward approach for isolating active constituents from P. cyrtonema Hua.
{"title":"An Efficient Method to Separate the Main Constituents From Polygonatum cyrtonema Hua by a Combination of Online-Storage Inner-Recycling and Consecutive High-Speed Counter-Current Chromatography","authors":"Kai Zhong, Yingjian Guo, Yuning Wang, Longsheng Guo, Lei Zhao, Tao Yue, Hui Wang, Jinqian Yu","doi":"10.1002/jssc.70329","DOIUrl":"https://doi.org/10.1002/jssc.70329","url":null,"abstract":"<div>\u0000 \u0000 <p>A novel strategy combining XAD-4 macroporous resin pretreatment and online-storage inner-recycling high-speed counter-current chromatography (OS-IRCCC) was developed for efficient separation of multi-polarity constituents from <i>Polygonatum cyrtonema</i> Hua. The innovation lies in the OS-IRCCC mode, which integrates online storage of target fractions via a six-way valve-equipped recycling loop and inner-recycling separation, overcoming limitations of conventional high-speed counter-current chromatography in resolving structurally similar compounds. After resin fractionation, 40%, 60%, and 95% ethanol eluates were separated using methyl tert-butyl ether/<i>n</i>-butanol/acetonitrile/water (1:4:1:5, v/v) solvent system, chloroform/methanol/water (7:6:4, v/v) solvent system (with OS-IRCCC for Compounds <b>8</b> and <b>9</b>), and petroleum ether/ethyl acetate/methanol/water (5:5:4:3, v/v) solvent system, respectively. Thirteen compounds were successfully isolated, including four high-polarity glycosides (<b>1</b>–<b>4</b>), five medium-polarity phenolic constituents (<b>5</b>–<b>9</b>), and four low-polarity terpenes (<b>10</b>–<b>13</b>). This study demonstrates that the established separation method provides an efficient, rapid, and straightforward approach for isolating active constituents from <i>P. cyrtonema</i> Hua.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 12","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-11-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145619368","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}
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