Journal of separation science最新文献

{"title":"Recent Advances in Sample Preparation for Cholesterol and Oxysterol Analysis in Complex Biological Matrices","authors":"Haizhen Zhang,&nbsp;Longchan Liu,&nbsp;Haoyue Zhang,&nbsp;Linnan Li,&nbsp;Zhengtao Wang,&nbsp;Li Yang","doi":"10.1002/jssc.70539","DOIUrl":"https://doi.org/10.1002/jssc.70539","url":null,"abstract":"<div>\u0000 \u0000 <p>Cholesterol and oxysterols are key molecules that regulate physiological processes and participate in the occurrence and progression of various major diseases. Accurate and efficient analytical detection of these substances in complex biological matrices is critical for disease mechanism research and biomarker discovery. However, challenges including complex biological matrices, large differences in analyte abundance, susceptibility to auto‑oxidation, low ionization efficiency, and difficulty in isomer separation pose severe obstacles to reliable analysis, making sample preparation the core step for accurate quantification and valid identification. Continuous innovations have been achieved in sample preparation techniques, such as liquid–liquid extraction, solid‑phase extraction, deep eutectic solvent extraction, molecularly imprinted extraction, derivatization, as well as integrated and automated workflows. These advances improve extraction efficiency, selectivity, antioxidant protection, and throughput, while effectively reducing matrix interference and artificial oxidation. This paper systematically reviews the research progress in sample preparation for cholesterol and oxysterol analysis in complex biological matrices from 2015 to 2026, highlights the technical advantages, application scenarios, and current limitations of various pretreatment strategies, and prospects the development trends toward greening, intelligence, and high throughput.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149146558","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":"Evaluation of a Hydrophilic Interaction Liquid Chromatography Design Space for Amino Acids","authors":"Laura K. Muehlbauer,&nbsp;Nahyr A. López Dauphin,&nbsp;Timothy T. Kramer,&nbsp;Alana Kurz,&nbsp;Donald S. Risley","doi":"10.1002/jssc.70547","DOIUrl":"https://doi.org/10.1002/jssc.70547","url":null,"abstract":"<div>\u0000 \u0000 <p>A column ranking system was developed for the separation of all 20 proteinogenic amino acids using hydrophilic interaction liquid chromatography mode across 18 polar stationary phases with acetonitrile/aqueous mobile phases. Each amino acid was individually evaluated on all columns using gradient elution, and the retention time data were compiled into a statistical ranking algorithm that enables selection of any analyte subset and identifies the column providing the greatest separation between successively eluting analytes. Since most of these analytes lack strong chromophores, evaporative light scattering detection was employed for quantitative detection. Mobile phase pH (3.5 to 6.0) and ammonium formate concentration (10 to 100 mM) were then optimized on the three highest-ranked columns (Accucore-150-Amide HILIC, TSKgel Amide-80, and Poroshell 120 HILIC-OH5). Retention of most amino acids was insensitive to pH, whereas arginine and lysine showed inverse dependence on buffer concentration compared with all other analytes, and 50 mM ammonium formate without pH adjustment gave the best compromise for the complete analyte set. Re-querying the ranking algorithm for smaller analyte subsets returned a different optimal column in each case, confirming that no single stationary phase is universally preferable. Knowledge gained from evaluating the design space facilitated the rapid development of a quantitative method for the determination of the amino acid composition of a capsule formulation. The isocratic assay was linear for leucine, isoleucine, and valine over approximately 0.1 to 1.0 mg/mL (<i>R</i>² ≥ 0.997), recovered 102%–104% of label claim across six independent preparations, and gave injection precision of ≤ 0.45% relative standard deviation with quantitation limits of ≤ 114 µg/mL.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149146573","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":"Evaluation of a Hydrophilic Interaction Liquid Chromatography Design Space for Amino Acids","authors":"Laura K. Muehlbauer,&nbsp;Nahyr A. López Dauphin,&nbsp;Timothy T. Kramer,&nbsp;Alana Kurz,&nbsp;Donald S. Risley","doi":"10.1002/jssc.70547","DOIUrl":"https://doi.org/10.1002/jssc.70547","url":null,"abstract":"<div>\u0000 \u0000 <p>A column ranking system was developed for the separation of all 20 proteinogenic amino acids using hydrophilic interaction liquid chromatography mode across 18 polar stationary phases with acetonitrile/aqueous mobile phases. Each amino acid was individually evaluated on all columns using gradient elution, and the retention time data were compiled into a statistical ranking algorithm that enables selection of any analyte subset and identifies the column providing the greatest separation between successively eluting analytes. Since most of these analytes lack strong chromophores, evaporative light scattering detection was employed for quantitative detection. Mobile phase pH (3.5 to 6.0) and ammonium formate concentration (10 to 100 mM) were then optimized on the three highest-ranked columns (Accucore-150-Amide HILIC, TSKgel Amide-80, and Poroshell 120 HILIC-OH5). Retention of most amino acids was insensitive to pH, whereas arginine and lysine showed inverse dependence on buffer concentration compared with all other analytes, and 50 mM ammonium formate without pH adjustment gave the best compromise for the complete analyte set. Re-querying the ranking algorithm for smaller analyte subsets returned a different optimal column in each case, confirming that no single stationary phase is universally preferable. Knowledge gained from evaluating the design space facilitated the rapid development of a quantitative method for the determination of the amino acid composition of a capsule formulation. The isocratic assay was linear for leucine, isoleucine, and valine over approximately 0.1 to 1.0 mg/mL (<i>R</i>² ≥ 0.997), recovered 102%–104% of label claim across six independent preparations, and gave injection precision of ≤ 0.45% relative standard deviation with quantitation limits of ≤ 114 µg/mL.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149146559","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":"In-situ Grown Covalent Organic Frameworks on Electrospun Nanofibers for Efficient Enrichment and Determination of Organophosphate Esters in Biodegradable Plastics","authors":"Xinrui Tian,&nbsp;Yao Wang,&nbsp;Jiayi Song,&nbsp;Ping Su,&nbsp;Yi Yang","doi":"10.1002/jssc.70551","DOIUrl":"10.1002/jssc.70551","url":null,"abstract":"<div>\u0000 \u0000 <p>In this work, a covalent organic framework (COF)-based nanofibrous composite (PAN@TFPB-TAPB) was fabricated through an in situ growth strategy and explored as a high-performance sorbent for thin film microextraction (TFME). Benefiting from the integration of electrospun polyacrylonitrile (PAN) nanofibers and TFPB-TAPB (2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde [TFPB] and 1,3,5-tris(4-aminophenylbenzene) [TAPB]), the composite mitigated the aggregation of conventional COF powders and provided accessible adsorption sites with good structural stability. The as-prepared PAN@TFPB-TAPB sorbent exhibited higher extraction efficiency toward seven organophosphate esters (OPEs) compared with pure PAN and TFPB-TAPB. On this basis, a sensitive and reliable TFME-gas chromatography-mass spectrometry method was established for the simultaneous enrichment and determination of OPEs in degradable plastic samples. Under the optimal conditions, the proposed method displayed wide linear ranges, low limits of detection, good precision, and satisfactory recoveries. Furthermore, this method was successfully applied to the analysis of OPEs in real complex plastic samples, demonstrating its great practical potential for the efficient monitoring of OPEs in environmental and commodity-related matrices.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149137289","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":"Green Sorptive Sampling Coupled With UHPLC–IMS–MS and GC×GC–TOFMS for Characterization of Migrating Substances From Plastic Food Contact Materials","authors":"Gizelle Roque van Niekerk,&nbsp;Yvette Naudé,&nbsp;Madelien Wooding","doi":"10.1002/jssc.70549","DOIUrl":"10.1002/jssc.70549","url":null,"abstract":"<p>Comprehensive analysis of migrating compounds from plastic food contact materials (FCMs) is analytically demanding due to the structural diversity and broad physicochemical properties of intentionally and non-intentionally added substances (IAS and NIAS). This necessitates the development of advanced, multidimensional separation techniques coupled with high-resolution detection for trace-level characterization. Five million tones of chemical additives are incorporated into plastic FCMs annually, which is concerning considering the health risks associated with human exposure to migrating chemicals. This study provides a simplified green sorptive sampling loop for detecting and quantifying IAS and NIAS that migrate from FCMs during everyday use. A polydimethylsiloxane (PDMS) sorptive sampler loop was used as the sampling device, allowing migrated compounds to be enriched directly from the sample matrix. After extraction, the same sampler format was compatible with two analytical workflows: thermal desorption directly into the GC inlet for GC×GC–TOFMS analysis, or liquid back-extraction into solvent for subsequent UHPLC-IMS-MS analysis. Complementary chromatography and ion mobility high-resolution mass spectrometry (UHPLC–IMS–MS and GC×GC–TOFMS) enabled the detection and quantification of a range of chemical compounds at trace levels, including phthalates, UV absorbers, stabilizers, surfactants, and hydrocarbons. Over 30 compounds were detected as migrating from FCMs using GC–MS, and 26 compounds were identified using LC–MS. Unknown target identification using LC–MS was aided by the use of collision cross section (CCS) values, thus strengthening putative identification. Limits of detection of the eight target analytes ranged from 0.023 to 97 ng L⁻¹ for LC–MS and IAS were detected at concentrations ranging from 0.0065 to ∼25 µg L^− 1. Our study exemplifies the wide range of chemical compounds that migrate from FCMs during everyday FCM use. The green sampling technique presented here allowed the quantification of daily exposure to these chemicals and has potential application to human health and environmental risk assessments.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70549","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149137248","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":"Modelling Retention Behavior Over Broad Ranges of Organic Modifier Concentrations in Reversed-Phase Liquid Chromatography Columns","authors":"Kristof Vynckier,&nbsp;Leon Niezen,&nbsp;Bram Huygens,&nbsp;Judith Mollen,&nbsp;Deirdre Cabooter,&nbsp;Gert Desmet","doi":"10.1002/jssc.70548","DOIUrl":"10.1002/jssc.70548","url":null,"abstract":"<div>\u0000 \u0000 <p>The present study aimed to investigate how complex an analytical retention time model needs to be to closely represent the strong curvature in the relation between the logarithm of the retention factor and the fraction of organic modifier <span></span><math>\u0000 <semantics>\u0000 <mi>ϕ</mi>\u0000 <annotation>$phi $</annotation>\u0000 </semantics></math> that is often observed when exploring broad ranges of <span></span><math>\u0000 <semantics>\u0000 <mi>ϕ</mi>\u0000 <annotation>$phi $</annotation>\u0000 </semantics></math>. This is, for example, the case during automated method development. It was found that, when covering wide <span></span><math>\u0000 <semantics>\u0000 <mi>ϕ</mi>\u0000 <annotation>$phi $</annotation>\u0000 </semantics></math>-ranges, 3-parameter models are essential to capture the curvature of <span></span><math>\u0000 <semantics>\u0000 <mrow>\u0000 <mi>ln</mi>\u0000 <mo>(</mo>\u0000 <mi>k</mi>\u0000 <mo>)</mo>\u0000 </mrow>\u0000 <annotation>$ln ( k )$</annotation>\u0000 </semantics></math> vs. <span></span><math>\u0000 <semantics>\u0000 <mi>ϕ</mi>\u0000 <annotation>$phi $</annotation>\u0000 </semantics></math> relations, with the Neue–Kuss (NK) and hybrid-log (HYL) models outperforming the standard quadratic model. However, moving to 4-parameter models still yielded a statistically significant improvement, as confirmed by the RMSE values (from 0.051 to 0.016 median) and the Akaike Information Criterion (AIC)-values (with ΔAIC &gt; 10), especially for data sets containing compounds that exhibited a retention minimum. Among these, two newly proposed models performed slightly better than the standard cubic model in both global fitting accuracy and high-<span></span><math>\u0000 <semantics>\u0000 <mi>k</mi>\u0000 <annotation>$k$</annotation>\u0000 </semantics></math> extrapolation accuracy. Even so, relatively large performance variance across all methods implied that important exceptions to these general trends exist.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149137331","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":"Heart‑Cutting Two‑Dimensional Liquid Chromatography/High‑Resolution Mass Spectrometry and Complementary High-Performance Liquid Chromatography Methods for Comprehensive Impurity Profiling and Quality Control of Dalbavancin Hydrochloride","authors":"Hongling Xu,&nbsp;Xinying Du,&nbsp;Jinjin Lv,&nbsp;Jing Liu,&nbsp;Xincheng Shen,&nbsp;Duxin Li","doi":"10.1002/jssc.70545","DOIUrl":"10.1002/jssc.70545","url":null,"abstract":"<div>\u0000 \u0000 <p>Dalbavancin hydrochloride (DB) is a semi‑synthetic lipoglycopeptide antibiotic whose pharmacopeial impurity analysis relies on mobile phases containing non‑volatile phosphate buffers. Although effective for separation, these buffers are incompatible with mass spectrometry (MS), impeding structural characterization of trace impurities. In this study, a heart‑cutting two‑dimensional liquid chromatography/high‑resolution MS (2D‑LC/HRMS) method was developed to overcome this limitation. The first dimension employed a dual‑column serial system with a phosphate‑based mobile phase to achieve high‑resolution separation of dalbavancin and its related substances. Target fractions were online transferred to a second dimension with MS‑compatible conditions for desalting and accurate mass analysis. Using this approach, 22 components—including five major components (DB‑A0, DB‑A1, DB‑B0, DB‑B1, and DB‑B2) and 17 impurities (e.g., DB‑R1, DB‑R2, DB‑D0, DB‑D1, DB‑C0, DB‑C1, RRT0.94, and RRT0.96)—were identified based on accurate mass and tandem MS fragmentation patterns, with confirmation by reference standards where available. To support routine quality control, three complementary high-performance LC methods were developed and fully validated according to ICH guidelines for the quantification of related substances, specific impurities DBa/RRT1.12/RRT1.15, and the highly polar impurity DB‑R6. Forced‑degradation studies under thermal, photolytic, acidic, alkaline, and oxidative conditions revealed distinct degradation behaviors: DB‑R1 increased markedly under thermal, acidic, and photolytic stress; DB‑R2 was the primary alkaline degradation product; DBa and RRT0.96 increased markedly under oxidative conditions; and DB‑R6 increased markedly under acidic conditions. This integrated analytical workflow provides a robust platform for both impurity characterization and routine quality control of DB, supporting process optimization and stability assessment.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-10-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149127887","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":"Enantioselective HPLC of Liquid Crystals Bearing a Small and Flexible 2-Methylbutyl Chiral Center","authors":"Terézia Jurkovičová,&nbsp;Martin Cigl,&nbsp;Věra Hamplová,&nbsp;Vladimíra Novotná,&nbsp;Petra Vaňkátová","doi":"10.1002/jssc.70552","DOIUrl":"10.1002/jssc.70552","url":null,"abstract":"<p>The conformationally flexible 2-methylbutyl structural motif represents a small chiral center, which cannot engage in polar interactions with chiral stationary phases (e.g., hydrogen bonds), which often play a key role in enantioselective recognition. In this contribution, racemic liquid crystalline materials sharing the 2-methylbutyl group were analyzed by enantioselective high-performance liquid chromatography, and the studied analyte set also included diastereomeric compounds with additional chiral centers based on the lactate unit. As the non-chiral parts of the analytes are rigid and bulky, this disbalance in size and flexibility further complicates enantioseparation of such materials. The separations were done under either polar organic mode or reversed-phase liquid chromatography conditions to enhance the less polar interactions with the chiral stationary phases. Two polysaccharide chiral stationary phases were employed—coated <i>tris</i>(5-chloro-2-methylcarbamate) amylose and immobilized <i>tris</i>(3-chloro-5-methylphenylcarbamate) amylose. Baseline enantioseparation of all racemic samples was accomplished in less than 9 minutes. Effects of analytes’ structural variations on enantioselectivity are discussed, and the differences between results on the two chiral stationary phases are assessed.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13643178/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149111330","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":"Computationally Guided Design of Magnetic Molecularly Imprinted Polymers for the Selective Determination of Pyrethroid Pesticides in Foods","authors":"Yiliu Zheng,&nbsp;Jingjing Li,&nbsp;Hua Shao,&nbsp;Yong Shao,&nbsp;Miao Wang,&nbsp;Juanxia Wang,&nbsp;Hailong Yu,&nbsp;Yongxin She,&nbsp;Jing Wang,&nbsp;A. M. Abd El-Aty","doi":"10.1002/jssc.70530","DOIUrl":"10.1002/jssc.70530","url":null,"abstract":"<div>\u0000 \u0000 <p>A magnetic molecularly imprinted polymer (MMIP) with high specificity for pyrethroid pesticides was successfully synthesized via a surface molecular imprinting strategy. Using fenvalerate as the template, density functional theory (DFT) calculations were performed to systematically evaluate four candidate functional monomers: methacrylic acid (MAA), acrylic acid (AA), 4-vinylpyridine (4-VP), and allyl-β-cyclodextrin (allyl-β-CD). Computational analyses revealed that allyl-β-CD yields a significantly increased imprinting factor, underscoring its superior capacity to confer adsorption selectivity. Binding energy calculations further elucidated the molecular recognition mechanism underlying the MMIP–template interaction. Comprehensive physicochemical characterization, including X-ray diffraction (XRD), scanning/transmission electron microscopy (SEM/TEM), and Fourier transform infrared spectroscopy (FT-IR), confirmed both the structural integrity and surface morphology of the resulting polymer. To demonstrate practical utility, MMIPs were employed in magnetic dispersive solid-phase extraction (MDSPE) for the simultaneous purification and enrichment of six pyrethroid pesticides (Pyrs) from apple and cabbage matrices. By coupling MDSPE with high-performance liquid chromatography‒tandem mass spectrometry (HPLC‒MS/MS), a robust analytical protocol was developed and validated for the determination of pyrethroid residues in fruits and vegetables. Recovery experiments across multiple fortification levels yielded mean recoveries of 72%–109%, with relative standard deviations (RSDs) of 0.65%–5.04%. This validated MDSPE–HPLC–MS/MS method provides a cost-effective and time-saving reliable analytical tool for routine monitoring of pyrethroid residues in fresh produce, contributing to improved food safety surveillance and regulatory compliance, and offering practical applicability for routine food safety monitoring laboratories.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149111382","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":"Chemical Profiling of Jiedu Huoxue Decoction by Ultra-High-Performance Liquid Chromatography Coupled With Q Exactive Orbitrap and Quantification of Main Effective Constituents by Triple Quadrupole Mass Spectrometry","authors":"Yanxin Wang,&nbsp;Le Yang,&nbsp;Huimin Lin,&nbsp;Fan He,&nbsp;Ye Sun,&nbsp;Ruimin Tian,&nbsp;Xiaowan Wang,&nbsp;Xijun Mu,&nbsp;Peng Xu","doi":"10.1002/jssc.70541","DOIUrl":"10.1002/jssc.70541","url":null,"abstract":"<div>\u0000 \u0000 <p>The Jiedu Huoxue decoction (JHD) is a traditional Chinese herbal formula used by Professor Zhang Qi, a Master of Traditional Chinese Medicine, to treat acute kidney injury, and it has demonstrated good clinical efficacy. However, existing studies lack a systematic characterization of the overall chemical composition of JHD and unified evaluation standards for its quality control. This situation hinders the comprehensive development and application of JHD in clinical practice, and its pharmacological mechanism has not been clarified. In this study, a rapid and sensitive ultra-high-performance liquid chromatography-Q Exactive Orbitrap mass spectrometry (UHPLC-Q-Exactive Orbitrap MS) technology was employed to rapidly analyze and identify the chemical constituents of JHD. High-resolution mass spectrometric data were acquired in Full MS/dd-MS² mode, with precursor ions fragmented by higher-energy collisional dissociation using stepped normalized collision energies of 20, 35, and 50. A total of 177 compounds were found, including 84 flavonoids, 23 terpenes, 23 phenylpropanoids, 10 triterpene saponins, nine phenethyl glycosides, nine glycosides, six amino acids, four fatty acids, three organic acids, and six other compounds. In addition, a comprehensive analytical strategy based on HPLC-QqQ-MS/MS was established, enabling rapid quantitative analysis of 16 active components in JHD within 15 min, which provides a scientific basis for quality control and effective component research of JHD.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 10","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149111318","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}