Journal of separation science最新文献

{"title":"Rapid and Selective Extraction and Detection of Baicalin From Scutellariae Radix Using Magnetic Molecularly Imprinted Polymers","authors":"Jing Li,&nbsp;Yihan Sun,&nbsp;Jialin Guo,&nbsp;Wei Zhao,&nbsp;Xia Liu","doi":"10.1002/jssc.70507","DOIUrl":"https://doi.org/10.1002/jssc.70507","url":null,"abstract":"<div>\u0000 \u0000 <p>Baicalin (BA), a key flavonoid isolated from <i>Scutellariae Radix</i> (<i>SR</i>), possesses diverse pharmacological activities encompassing anticancer, anti-inflammatory, and hepatoprotective effects. In order to achieve rapid separation and enrichment of BA from complex matrix samples, core–shell magnetic molecularly imprinted polymers (MMIPs) were fabricated using BA as the template molecule and Fe₃O₄ nanoparticles as the magnetic core. Subsequently, key preparation parameters, including the ratio of functional monomers to cross-linking agents, imprinting time, and the dosage of BA were systematically optimized. Under the optimized conditions, the prepared MMIPs exhibited rapid binding kinetics and a remarkable maximum adsorption capacity of 18.21 mg/g, accompanied by an imprinting factor (IF) of 3.919. Furthermore, the developed MMIPs were successfully employed for the selective extraction and determination of BA from <i>SR</i>. Specifically, the average recoveries of BA at three spiked concentrations (5.00, 11.20, and 20.00 µg/mL) were 107.0%, 92.7%, and 105.2%, respectively, with corresponding relative standard deviations (RSDs) of 5.31%, 1.65%, and 3.28% (<i>n</i> = 3). Overall, this work provides a novel and efficient adsorbent for trace flavonoids enrichment from complex herbal samples, offering a promising pretreatment strategy for active ingredient analysis in traditional Chinese medicine research.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148784962","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":"Discovery of Cardioprotective Markers in Huangqi Shengmai Yin via Integrated UHPLC-Q-TOF-MS/MS Fingerprinting, Chemometric Quality Assessment, and Bioactivity Correlation","authors":"Peijing Jiang,&nbsp;Yacheng Lv,&nbsp;Jie Zhang,&nbsp;Yangsheng Chen,&nbsp;Zhuoying Jin,&nbsp;Xiangqun Lv,&nbsp;Yanxia Lv,&nbsp;Yi Tao","doi":"10.1002/jssc.70509","DOIUrl":"https://doi.org/10.1002/jssc.70509","url":null,"abstract":"<div>\u0000 \u0000 <p>Huangqi Shengmai Yin (HQSMY) displays notable cardioprotective properties. Nevertheless, the principal pharmacodynamic constituents underpinning this efficacy have not yet been fully clarified. To tackle this issue, an integrative workflow coupling UHPLC‑Q‑TOF‑MS/MS fingerprinting, chemometrics, and spectrum‑effect correlations was constructed for the systematic discovery of cardioprotective markers. Fifty-one components from 10 batches of HQSMY samples were characterized by UHPLC‑Q‑TOF‑MS/MS in conjunction with the GNPS molecular networking platform. Subsequently, chromatographic fingerprints were established, with 22 and 29 characteristic common peaks assigned in negative and positive ion modes, respectively. Interbatch consistency was assessed via chemometric methods. Spectrum‑effect relationship analyses were conducted through Pearson correlation, gray relational analysis, and OPLS regression, revealing that formononetin, astrapterocarpan, astragaloside II, schisandrin, and biochanin A exhibited highly significant positive correlations with H9c2 cardiomyocyte protective activity. All these compounds attained gray relational scores exceeding 0.7, implying strong associations with cardioprotective action. These five components were then chosen from the candidate markers for subsequent functional validation using the CCK-8 assay, which yielded EC₅₀ values of 18.60 ± 3.15 µM (biochanin A), 26.42 ± 4.78 µM (formononetin), 92.93 ± 19.14 µM (astragaloside II), 70.85 ± 13.26 µM (schisandrin), and 72.73 ± 14.05 µM (astrapterocarpan). The cardioprotective effect of astragaloside II, schisandrin, and astrapterocarpan in H₂O₂-induced H9c2 injury model were reported for the first time. This integrated analytical strategy not only pinpoints the primary cardioprotective components of HQSMY but also furnishes a dependable methodological framework for quality evaluation and pharmacodynamic material research.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783846","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Rapid and Selective Extraction and Detection of Baicalin From Scutellariae Radix Using Magnetic Molecularly Imprinted Polymers","authors":"Jing Li,&nbsp;Yihan Sun,&nbsp;Jialin Guo,&nbsp;Wei Zhao,&nbsp;Xia Liu","doi":"10.1002/jssc.70507","DOIUrl":"https://doi.org/10.1002/jssc.70507","url":null,"abstract":"<div>\u0000 \u0000 <p>Baicalin (BA), a key flavonoid isolated from <i>Scutellariae Radix</i> (<i>SR</i>), possesses diverse pharmacological activities encompassing anticancer, anti-inflammatory, and hepatoprotective effects. In order to achieve rapid separation and enrichment of BA from complex matrix samples, core–shell magnetic molecularly imprinted polymers (MMIPs) were fabricated using BA as the template molecule and Fe₃O₄ nanoparticles as the magnetic core. Subsequently, key preparation parameters, including the ratio of functional monomers to cross-linking agents, imprinting time, and the dosage of BA were systematically optimized. Under the optimized conditions, the prepared MMIPs exhibited rapid binding kinetics and a remarkable maximum adsorption capacity of 18.21 mg/g, accompanied by an imprinting factor (IF) of 3.919. Furthermore, the developed MMIPs were successfully employed for the selective extraction and determination of BA from <i>SR</i>. Specifically, the average recoveries of BA at three spiked concentrations (5.00, 11.20, and 20.00 µg/mL) were 107.0%, 92.7%, and 105.2%, respectively, with corresponding relative standard deviations (RSDs) of 5.31%, 1.65%, and 3.28% (<i>n</i> = 3). Overall, this work provides a novel and efficient adsorbent for trace flavonoids enrichment from complex herbal samples, offering a promising pretreatment strategy for active ingredient analysis in traditional Chinese medicine research.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783845","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":"Discovery of Cardioprotective Markers in Huangqi Shengmai Yin via Integrated UHPLC-Q-TOF-MS/MS Fingerprinting, Chemometric Quality Assessment, and Bioactivity Correlation","authors":"Peijing Jiang,&nbsp;Yacheng Lv,&nbsp;Jie Zhang,&nbsp;Yangsheng Chen,&nbsp;Zhuoying Jin,&nbsp;Xiangqun Lv,&nbsp;Yanxia Lv,&nbsp;Yi Tao","doi":"10.1002/jssc.70509","DOIUrl":"https://doi.org/10.1002/jssc.70509","url":null,"abstract":"<div>\u0000 \u0000 <p>Huangqi Shengmai Yin (HQSMY) displays notable cardioprotective properties. Nevertheless, the principal pharmacodynamic constituents underpinning this efficacy have not yet been fully clarified. To tackle this issue, an integrative workflow coupling UHPLC‑Q‑TOF‑MS/MS fingerprinting, chemometrics, and spectrum‑effect correlations was constructed for the systematic discovery of cardioprotective markers. Fifty-one components from 10 batches of HQSMY samples were characterized by UHPLC‑Q‑TOF‑MS/MS in conjunction with the GNPS molecular networking platform. Subsequently, chromatographic fingerprints were established, with 22 and 29 characteristic common peaks assigned in negative and positive ion modes, respectively. Interbatch consistency was assessed via chemometric methods. Spectrum‑effect relationship analyses were conducted through Pearson correlation, gray relational analysis, and OPLS regression, revealing that formononetin, astrapterocarpan, astragaloside II, schisandrin, and biochanin A exhibited highly significant positive correlations with H9c2 cardiomyocyte protective activity. All these compounds attained gray relational scores exceeding 0.7, implying strong associations with cardioprotective action. These five components were then chosen from the candidate markers for subsequent functional validation using the CCK-8 assay, which yielded EC₅₀ values of 18.60 ± 3.15 µM (biochanin A), 26.42 ± 4.78 µM (formononetin), 92.93 ± 19.14 µM (astragaloside II), 70.85 ± 13.26 µM (schisandrin), and 72.73 ± 14.05 µM (astrapterocarpan). The cardioprotective effect of astragaloside II, schisandrin, and astrapterocarpan in H₂O₂-induced H9c2 injury model were reported for the first time. This integrated analytical strategy not only pinpoints the primary cardioprotective components of HQSMY but also furnishes a dependable methodological framework for quality evaluation and pharmacodynamic material research.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148784405","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":"Aerogel Pore-Confined High-Loading MOF-199 for Micro-Solid-Phase Extraction of Methorphan Enantiomer in Biological Samples","authors":"Shaojing Huang,&nbsp;Suling Zhang,&nbsp;Huanhuan Yao,&nbsp;Zhiwei Huang,&nbsp;Dong Zhang,&nbsp;Ying Pan,&nbsp;Ting Lü,&nbsp;Hongting Zhao","doi":"10.1002/jssc.70506","DOIUrl":"https://doi.org/10.1002/jssc.70506","url":null,"abstract":"<div>\u0000 \u0000 <p>Dextromethorphan is a widely used clinical antitussive, while its enantiomer, levomethorphan, is a controlled substance. Chiral separation and trace detection of the two enantiomers in biological samples are critically important. Herein, a micro-solid-phase extraction method coupled with enantioselective ultra-high performance liquid chromatography–mass spectrometry (UHPLC–MS) was proposed for the analysis of methorphan enantiomers. MOF-199/cellulose aerogel spheres fabricated via a facile in situ growth strategy were employed as the sorbent. By immersing Cu²⁺-rich cellulose aerogel in H₃BTC (1,3,5-benzene tricarboxylate) solutions at varied concentrations, MOF-199/cellulose aerogels with tunable MOF-199 loadings (28.8%, 38.1%, 43.8%) were fabricated. Characterization results verified that MOF-199 was uniformly anchored in the pore channels of cellulose aerogel, which not only enhanced its specific surface area from 33.9 to 143.6 m²/g, but also mitigated the aggregation and poor recyclability of powdered MOF-199. The electrostatic attraction, chelation, and hydrogen-bonding interactions accounted for the effective extraction for dextro- and levo-methorphan. Under optimized conditions, this method exhibited favorable linearity in the range of 0.02–10.0 µg/L, with intra- and inter-day precisions of 4.9%–5.0% and 7.7%–9.7%, respectively. The limits of detection were 0.01–0.02 µg/L, respectively. Recoveries of dextro- and levo-methorphan from urine and hair samples were in the ranges of 88.9%–119.3% and 78.6%–115.7%, respectively. This method provides an effective strategy for the determination of methorphan enantiomers in biological samples, featuring rapid pretreatment, low organic solvent consumption, as well as facile operation.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148784178","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":"Aerogel Pore-Confined High-Loading MOF-199 for Micro-Solid-Phase Extraction of Methorphan Enantiomer in Biological Samples","authors":"Shaojing Huang,&nbsp;Suling Zhang,&nbsp;Huanhuan Yao,&nbsp;Zhiwei Huang,&nbsp;Dong Zhang,&nbsp;Ying Pan,&nbsp;Ting Lü,&nbsp;Hongting Zhao","doi":"10.1002/jssc.70506","DOIUrl":"https://doi.org/10.1002/jssc.70506","url":null,"abstract":"<div>\u0000 \u0000 <p>Dextromethorphan is a widely used clinical antitussive, while its enantiomer, levomethorphan, is a controlled substance. Chiral separation and trace detection of the two enantiomers in biological samples are critically important. Herein, a micro-solid-phase extraction method coupled with enantioselective ultra-high performance liquid chromatography–mass spectrometry (UHPLC–MS) was proposed for the analysis of methorphan enantiomers. MOF-199/cellulose aerogel spheres fabricated via a facile in situ growth strategy were employed as the sorbent. By immersing Cu²⁺-rich cellulose aerogel in H₃BTC (1,3,5-benzene tricarboxylate) solutions at varied concentrations, MOF-199/cellulose aerogels with tunable MOF-199 loadings (28.8%, 38.1%, 43.8%) were fabricated. Characterization results verified that MOF-199 was uniformly anchored in the pore channels of cellulose aerogel, which not only enhanced its specific surface area from 33.9 to 143.6 m²/g, but also mitigated the aggregation and poor recyclability of powdered MOF-199. The electrostatic attraction, chelation, and hydrogen-bonding interactions accounted for the effective extraction for dextro- and levo-methorphan. Under optimized conditions, this method exhibited favorable linearity in the range of 0.02–10.0 µg/L, with intra- and inter-day precisions of 4.9%–5.0% and 7.7%–9.7%, respectively. The limits of detection were 0.01–0.02 µg/L, respectively. Recoveries of dextro- and levo-methorphan from urine and hair samples were in the ranges of 88.9%–119.3% and 78.6%–115.7%, respectively. This method provides an effective strategy for the determination of methorphan enantiomers in biological samples, featuring rapid pretreatment, low organic solvent consumption, as well as facile operation.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783991","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":"Integrated Liquid Chromatography-Tandem Mass Spectrometry and Headspace Solid-Phase Microextraction With Gas Chromatography-Mass Spectrometry-based Profiling Reveals Developmental Metabolic Dynamics of Ligusticum striatum DC.","authors":"Ninh Khac Thanh Tung,&nbsp;Nguyen Hoai Nam,&nbsp;Nguyen Xuan Nhiem,&nbsp;Nguyen Tien Dat,&nbsp;Sung Won Kwon,&nbsp;Jong Seong Kang,&nbsp;Hyung Min Kim","doi":"10.1002/jssc.70502","DOIUrl":"https://doi.org/10.1002/jssc.70502","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Ligusticum striatum</i> DC. (<i>Ligusticum chuanxiong</i> Hort. or <i>Ligusticum wallichii</i>) is a traditional medicinal herb in East Asia used for cardiovascular, neurological, and inflammatory disorders, but developmental phytochemical changes remain unclear. Here, targeted liquid chromatography-tandem mass spectrometry (LC-MS/MS) and untargeted headspace solid-phase microextraction with gas chromatography-MS were applied to examine five bioactive compounds and volatile organic compounds (VOCs) in aerial and root tissues across seven growth periods. Five compounds, including ferulic acid, icariside F2, ligusticoside A, <i>N</i>-3-(3-methoxy-4-hydroxyphenyl) allyl pipecolic acid, and ligustiphenol, were quantified with excellent linearity, sensitivity, precision, and accuracy. VOC profiling identified 33 and 32 compounds in aerial parts and roots, respectively, showing clear period- and tissue-specific differences. Chemometrics analysis revealed distinct clustering by growth stage, indicating dynamic metabolic shifts. Overall, roots served as reservoirs of phenolic acids, while aerial parts were enriched in phthalides and sesquiterpenes. These findings provide a basis for harvest optimization, quality control, and standardization of <i>L. striatum</i>, while novel compounds in Vietnamese herbal medicines expand its phytochemical diversity and pharmacological potential.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148784106","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":"Integrated Liquid Chromatography-Tandem Mass Spectrometry and Headspace Solid-Phase Microextraction With Gas Chromatography-Mass Spectrometry-based Profiling Reveals Developmental Metabolic Dynamics of Ligusticum striatum DC.","authors":"Ninh Khac Thanh Tung,&nbsp;Nguyen Hoai Nam,&nbsp;Nguyen Xuan Nhiem,&nbsp;Nguyen Tien Dat,&nbsp;Sung Won Kwon,&nbsp;Jong Seong Kang,&nbsp;Hyung Min Kim","doi":"10.1002/jssc.70502","DOIUrl":"https://doi.org/10.1002/jssc.70502","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Ligusticum striatum</i> DC. (<i>Ligusticum chuanxiong</i> Hort. or <i>Ligusticum wallichii</i>) is a traditional medicinal herb in East Asia used for cardiovascular, neurological, and inflammatory disorders, but developmental phytochemical changes remain unclear. Here, targeted liquid chromatography-tandem mass spectrometry (LC-MS/MS) and untargeted headspace solid-phase microextraction with gas chromatography-MS were applied to examine five bioactive compounds and volatile organic compounds (VOCs) in aerial and root tissues across seven growth periods. Five compounds, including ferulic acid, icariside F2, ligusticoside A, <i>N</i>-3-(3-methoxy-4-hydroxyphenyl) allyl pipecolic acid, and ligustiphenol, were quantified with excellent linearity, sensitivity, precision, and accuracy. VOC profiling identified 33 and 32 compounds in aerial parts and roots, respectively, showing clear period- and tissue-specific differences. Chemometrics analysis revealed distinct clustering by growth stage, indicating dynamic metabolic shifts. Overall, roots served as reservoirs of phenolic acids, while aerial parts were enriched in phthalides and sesquiterpenes. These findings provide a basis for harvest optimization, quality control, and standardization of <i>L. striatum</i>, while novel compounds in Vietnamese herbal medicines expand its phytochemical diversity and pharmacological potential.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148783544","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":"Development and Validation of a QuEChERS–LC–MS/MS Method for Simultaneous Determination of Four Direct Oral Anticoagulants in Citrate Plasma and Quantitative Dried Plasma Spots","authors":"Arkadiusz Kocur","doi":"10.1002/jssc.70505","DOIUrl":"https://doi.org/10.1002/jssc.70505","url":null,"abstract":"<div>\u0000 \u0000 <p>Direct oral anticoagulants (DOACs), including apixaban, dabigatran, edoxaban, and rivaroxaban, may require quantitative measurement in selected clinical situations despite fixed-dose administration. This study developed and validated a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-assisted liquid chromatography-tandem mass spectrometry method for their simultaneous determination in citrate plasma and quantitative dried plasma spot (qDPS) samples. Chromatographic separation was achieved on a Kinetex PS C18 column using a 4.0 min gradient, followed by positive electrospray ionization and scheduled multiple reaction monitoring. Sample preparation was optimized by comparing acetonitrile (ACN) protein precipitation, unbuffered and citrate-buffered QuEChERS extraction salts, and dispersive solid-phase extraction clean-up using primary-secondary amine, C18, EMR Lipid, Z-Sep+, or their combinations. The final procedure comprised ACN extraction with MgSO₄, NaCl, and Bond Elut EMR Lipid, followed by clean-up with MgSO₄, primary-secondary amine, and Z-Sep+. ACN provided the most consistent recovery across analytes, concentration levels, and matrices. The method was validated in accordance with International Council for Harmonization M10 using commercial plasma calibrators and independently prepared quality-control samples. Accuracy and precision met the predefined acceptance criteria in both matrices. Mean recovery ranged from 84.2% to 91.2% in citrate plasma and from 79.6% to 87.8% in dried plasma samples. Internal standard-normalized matrix factors ranged from 0.87 to 0.98, indicating limited ion suppression after the optimized clean-up procedure. External verification using materials from two independent proficiency-testing providers showed satisfactory agreement with assigned target values, with all results falling within the providers’ acceptance ranges. The method provides a robust QuEChERS-assisted workflow for the quantitative determination of DOACs in conventional citrate plasma and qDPS samples. Its clinical interchangeability between matrices requires further evaluation using paired patient samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148754179","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":"Development and Validation of a QuEChERS–LC–MS/MS Method for Simultaneous Determination of Four Direct Oral Anticoagulants in Citrate Plasma and Quantitative Dried Plasma Spots","authors":"Arkadiusz Kocur","doi":"10.1002/jssc.70505","DOIUrl":"https://doi.org/10.1002/jssc.70505","url":null,"abstract":"<div>\u0000 \u0000 <p>Direct oral anticoagulants (DOACs), including apixaban, dabigatran, edoxaban, and rivaroxaban, may require quantitative measurement in selected clinical situations despite fixed-dose administration. This study developed and validated a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-assisted liquid chromatography-tandem mass spectrometry method for their simultaneous determination in citrate plasma and quantitative dried plasma spot (qDPS) samples. Chromatographic separation was achieved on a Kinetex PS C18 column using a 4.0 min gradient, followed by positive electrospray ionization and scheduled multiple reaction monitoring. Sample preparation was optimized by comparing acetonitrile (ACN) protein precipitation, unbuffered and citrate-buffered QuEChERS extraction salts, and dispersive solid-phase extraction clean-up using primary-secondary amine, C18, EMR Lipid, Z-Sep+, or their combinations. The final procedure comprised ACN extraction with MgSO₄, NaCl, and Bond Elut EMR Lipid, followed by clean-up with MgSO₄, primary-secondary amine, and Z-Sep+. ACN provided the most consistent recovery across analytes, concentration levels, and matrices. The method was validated in accordance with International Council for Harmonization M10 using commercial plasma calibrators and independently prepared quality-control samples. Accuracy and precision met the predefined acceptance criteria in both matrices. Mean recovery ranged from 84.2% to 91.2% in citrate plasma and from 79.6% to 87.8% in dried plasma samples. Internal standard-normalized matrix factors ranged from 0.87 to 0.98, indicating limited ion suppression after the optimized clean-up procedure. External verification using materials from two independent proficiency-testing providers showed satisfactory agreement with assigned target values, with all results falling within the providers’ acceptance ranges. The method provides a robust QuEChERS-assisted workflow for the quantitative determination of DOACs in conventional citrate plasma and qDPS samples. Its clinical interchangeability between matrices requires further evaluation using paired patient samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148753498","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}