Journal of separation science最新文献

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Quantitative Analysis and Network Pharmacology-Based Profiling of Isolated Metabolites from Swertia purpurascens (D.Don) C.B. Clarke 紫癜獐牙菜(Swertia purpurascens)代谢物的定量分析和网络药理学分析。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-08-13 DOI: 10.1002/jssc.70498
Km Swati, Nitin Kumar, Taniya Sharma, Pooja Bhatt, Pamita Bhandari
{"title":"Quantitative Analysis and Network Pharmacology-Based Profiling of Isolated Metabolites from Swertia purpurascens (D.Don) C.B. Clarke","authors":"Km Swati,&nbsp;Nitin Kumar,&nbsp;Taniya Sharma,&nbsp;Pooja Bhatt,&nbsp;Pamita Bhandari","doi":"10.1002/jssc.70498","DOIUrl":"10.1002/jssc.70498","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Swertia purpurascens</i> is an important ethno-medicinal herb used for treating fever and colds. Despite its significance, the phytochemical profile of this species remains unexplored. This study aims to conduct a phytochemical investigation, develop a green and reliable analytical method assessing 11 specialized metabolites of <i>S. purpurascens</i>, and identify their suitable biological targets via network pharmacology. Among isolated metabolites, 3-hydroxybenzyl-β-<span>d</span>-glucopyranoside (<b>1</b>) has been reported for the first time from the <i>Swertia</i> genus, whereas compounds gentiopicroside (<b>2</b>), 1-hydroxy-3,5-dimethoxyxanthone (<b>5</b>), and methylswertianin (<b>6</b>) have been isolated for the first time from <i>S. purpurascens</i>. The developed method showed good linearity, sensitivity, precision, accuracy, and a positive green analytical profile. Results revealed that the stem part was the major source of metabolites (Yield: 125.70 ± 1.79 mg/g), compared with the other analyzed parts (flowers, leaves, and roots). Compounds <b>2</b> (0.72%–6.94%), <b>9</b> (0.08%–5.61%), and <b>1</b> (0.07%–2.71%) were quantified as the major compounds among different plant parts. Furthermore, network pharmacology analysis predicted the potential therapeutic relevance of these compounds with suggested pathways related to diabetes and cancer diseases. This study represents the first attempt to simultaneously quantify 11 specialized metabolites of <i>S. purpurascens</i> and to perform a network pharmacology-based analysis, thereby enriching its phytochemical understanding.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148721280","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}
引用次数: 0
pH-Regulated Reversible Phase Transition of Natural Deep Eutectic Solvents and Its Application in the Extraction of Fluorinated Liquid Crystal Monomers 天然深共晶溶剂ph调节可逆相变及其在含氟液晶单体萃取中的应用。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-08-12 DOI: 10.1002/jssc.70493
Ying Shao, Xiaoyan Jiang, Mengtao Jin, Xuerong Yang, Zuguang Li, Jinsong Liu
{"title":"pH-Regulated Reversible Phase Transition of Natural Deep Eutectic Solvents and Its Application in the Extraction of Fluorinated Liquid Crystal Monomers","authors":"Ying Shao,&nbsp;Xiaoyan Jiang,&nbsp;Mengtao Jin,&nbsp;Xuerong Yang,&nbsp;Zuguang Li,&nbsp;Jinsong Liu","doi":"10.1002/jssc.70493","DOIUrl":"10.1002/jssc.70493","url":null,"abstract":"<div>\u0000 \u0000 <p>Fluorinated liquid crystal monomers (FLCMs) are widely used in various electronic materials owing to their outstanding optoelectronic properties. However, their persistence, bioaccumulation, and toxicity, such as endocrine disruption, in the environment have rendered them emerging contaminants of significant concern. Switchable natural deep eutectic solvents (SNADESs) are prepared from natural compounds and their metabolites. These solvents possess the characteristics of green solvents while overcoming many limitations of conventional organic solvents, and have thus been widely adopted in the analysis and detection of environmental pollutants. In this study, a pH-SNADES was utilized as the extraction medium. Combined with ultrasound-assisted homogeneous liquid-liquid microextraction, a method for the extraction of FLCMs from environmental water samples was established, and the target analytes were qualitatively and quantitatively determined by gas chromatography-mass spectrometry. The results demonstrated that five of these compounds exhibited excellent linearity in the range of 0.5-500 ng mL<sup>−1</sup>, while the other two (4-(3,4-difluorophenyl)-4'-pentyl-1,1'-bi(cyclohexyl) and 3,4,5-trifluoro-4'-(4-pentylcyclohexyl)biphenyl) showed linearity in the range of 1-500 ng mL<sup>−1</sup>, with limits of detection ranging from 0.001 to 0.167 ng mL<sup>−1</sup> and limits of quantification ranging from 0.003 to 0.556 ng mL<sup>−1</sup>. Applied to real water samples, the method yielded spiked recoveries of 80.79%-125.42%, relative standard deviations of 0.09%-5.14%, and enrichment factors of 8-26, with its greenness and applicability further validated by three greenness assessment tools. The proposed method is efficient, environmentally friendly, and features mild reaction conditions and simple operation, providing technical support for the detection of FLCMs in environmental water samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148712790","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}
引用次数: 0
Discovery of Pancreatic Lipase Inhibitory and Antimicrobial Constituents in Crataegi Folium by High-Performance Thin-Layer Chromatography-Bioautography-Mass Spectrometry 高效薄层色谱-生物签名-质谱联用技术发现山楂叶中抑制胰腺脂肪酶及抗菌成分。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-08-11 DOI: 10.1002/jssc.70497
Liang Zhu, An-Lu Ma, Yi-Lian Zhang, Zi-Hao Si, Li-Hua Gu, Lin-Nan Li, Li Yang, Zheng-Tao Wang
{"title":"Discovery of Pancreatic Lipase Inhibitory and Antimicrobial Constituents in Crataegi Folium by High-Performance Thin-Layer Chromatography-Bioautography-Mass Spectrometry","authors":"Liang Zhu,&nbsp;An-Lu Ma,&nbsp;Yi-Lian Zhang,&nbsp;Zi-Hao Si,&nbsp;Li-Hua Gu,&nbsp;Lin-Nan Li,&nbsp;Li Yang,&nbsp;Zheng-Tao Wang","doi":"10.1002/jssc.70497","DOIUrl":"10.1002/jssc.70497","url":null,"abstract":"<div>\u0000 \u0000 <p>Crataegi Folium (CF), a traditional Chinese medicine widely used for promoting blood circulation and regulating lipid metabolism, contains diverse bioactive constituents with potential health-promoting effects. However, the rapid localization and identification of its functional compounds remain challenging due to the complexity of its chemical constituents. This study aimed to establish an integrated approach using high-performance thin-layer chromatography (HPTLC) coupled with bioactivity assay and mass spectrometry (MS) for the rapid screening and identification of pancreatic lipase inhibitory and antibacterial constituents in CF. Two HPTLC developing systems with different polarity ranges were optimized to comprehensively separate the chemical constituents, enabling effect-directed analysis. The results revealed that the pancreatic lipase inhibitory activity originated primarily from low-polarity triterpenoids. One active zone, consisting of co-migrating isomers, was successfully separated by in-situ iodine derivatization and characterized as maslinic acid and corosolic acid through comparison with reference standards. Another active zone was identified as arjunolic acid by using the exclusion method. Based on the <i>Vibrio fischeri</i> bioassay, six observed <i>V. fischeri</i> bioluminescence-inhibitory zones were mainly associated with high-polarity compounds, among which five were identified as isoquercitrin, hyperoside, chlorogenic acid, vitexin-2′′-O-rhamnoside, and vitexin-4′′-O-glucoside. Our findings provide new insights into bioactive constituents of CF, and demonstrate that HPTLC-bioautography-MS is an efficient and integrated platform for the rapid discovery and identification of markers for quality assessment of bioactive compounds in complex botanical matrices.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148707018","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}
引用次数: 0
Predicting the Aqueous Solubility of Neutral Organic Compounds by Reversed-Phase Liquid Chromatography 用反相液相色谱法预测中性有机化合物的水溶性。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-08-07 DOI: 10.1002/jssc.70504
Sanka N. Atapattu, Jianwei Li
{"title":"Predicting the Aqueous Solubility of Neutral Organic Compounds by Reversed-Phase Liquid Chromatography","authors":"Sanka N. Atapattu,&nbsp;Jianwei Li","doi":"10.1002/jssc.70504","DOIUrl":"10.1002/jssc.70504","url":null,"abstract":"<div>\u0000 \u0000 <p>Accurate estimation of water solubility is crucial for chemical screening, yet traditional predictive tools such as the General Solubility Equation (GSE) require melting point and octanol-water partition coefficient data and often struggle with weak electrolytes. This study presents two highly efficient reversed-phase liquid chromatography (RPLC) correlation strategies evaluated, comprising 49 binary solvent systems on three stationary phases. First, simple, melting point, octanol-water partition coefficient, and descriptor-free, isocratic models were explored to estimate the water solubility of neutral organic compounds using RPLC retention as the sole input. This approach demonstrated superior predictive accuracy of 0.307 log units and a more uniform error distribution across both non-electrolytes and weak electrolytes than the more conventional GSE. Second, to improve the predictive accuracy of estimating water solubility, RPLC retention and melting point data were explored. Predictive accuracy improved notably at higher organic volume fractions (50%–70% v/v) across all evaluated stationary phases. The correlation model comprising 70% (v/v) acetonitrile on an XTerra MS C18 stationary phase yielded a coefficient of determination of 0.962, a standard deviation of the model fit of 0.276, and an average absolute error value of 0.222. Together, these complementary chromatographic modelling strategies offer powerful, high-throughput alternatives for rapid solubility screening: providing either a direct, descriptor-free approach for compounds lacking structural information or a highly precise RPLC model approach combining retention and melting point data that minimizes prediction errors below 0.3 log units.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148685006","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}
引用次数: 0
Fabrication of Lead-based Metal-Organic Frameworks Using Recovered Lead for Solid-Phase Microextraction of p-Phenylenediamine Antioxidants 利用回收铅制备铅基金属有机骨架用于固相微萃取对苯二胺抗氧化剂。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-08-07 DOI: 10.1002/jssc.70499
Long Pang, Weiwei Yuan, Xingru Hu, Shujie Tang, Jia Wei
{"title":"Fabrication of Lead-based Metal-Organic Frameworks Using Recovered Lead for Solid-Phase Microextraction of p-Phenylenediamine Antioxidants","authors":"Long Pang,&nbsp;Weiwei Yuan,&nbsp;Xingru Hu,&nbsp;Shujie Tang,&nbsp;Jia Wei","doi":"10.1002/jssc.70499","DOIUrl":"10.1002/jssc.70499","url":null,"abstract":"<div>\u0000 \u0000 <p>The recycling of waste lead-acid batteries and the sensitive detection of trace <i>p</i>-phenylenediamine (PPD) antioxidants represent two pressing challenges in resource recovery and environmental safety. Herein, an integrated solution was proposed by synthesizing a novel lead-based metal-organic framework (WLP-Pb-MOF) from waste lead paste (WLP) as a sustainable metal source. The material served as a coating for a solid-phase microextraction (SPME) fiber. When coupled with gas chromatography-mass spectrometry, it enabled a highly sensitive method for determining three PPDs in water samples. The unique slit-shaped pore architecture and hydrophobic surface of WLP-Pb-MOF facilitated efficient enrichment through synergistic interactions, including size-sieving, hydrophobic partitioning, π-π stacking, and hydrogen bonding. This synergy resulted in extraction efficiencies significantly outperforming commercial SPME fibers. The method demonstrated good linearity from 5 to 2000 ng L<sup>−1</sup>, with detection limits of 0.29–1.60 ng L<sup>−1</sup>. In real water samples, the method achieved spiked recoveries of 91.3%–108.5%, with relative standard deviations below 8.78%. These results confirmed its accuracy and practical reliability. This work not only presents a viable strategy for the value-added recycling of waste lead but also provides a robust analytical platform for monitoring trace organic pollutants, effectively bridging sustainable resource recovery with advanced environmental monitoring.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148684973","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}
引用次数: 0
Are Microextraction Techniques Truly Green? A Critical Assessment of Green Sample Preparation Practices 微萃取技术真的环保吗?绿色样品制备实践的关键评估。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-07-31 DOI: 10.1002/jssc.70492
Rafael O. Martins, Maria F. A. Magalhães, Fernando M. Lanças
{"title":"Are Microextraction Techniques Truly Green? A Critical Assessment of Green Sample Preparation Practices","authors":"Rafael O. Martins,&nbsp;Maria F. A. Magalhães,&nbsp;Fernando M. Lanças","doi":"10.1002/jssc.70492","DOIUrl":"10.1002/jssc.70492","url":null,"abstract":"<div>\u0000 \u0000 <p>The development of sample preparation methods has led to smaller versions of traditional solid- and liquid-based techniques. This trend aims to align these methods with green analytical chemistry principles by reducing sample and solvent use and enabling more flexible designs, including online and automated systems. However, although miniaturization is often linked to environmental benefits, it also presents significant issues that are sometimes overlooked. These include the continued use of toxic solvents, labor-intensive procedures, and potential health and environmental risks that may be underestimated in the pursuit of “green” solutions. Therefore, this review offers a comprehensive and current overview of both solid- and liquid-based miniaturized techniques, emphasizing their environmental challenges. It focuses on balancing analytical performance with core green chemistry principles. Selected examples from recent literature highlight current applications and trends. Additionally, we discuss emerging directions and ongoing challenges that must be addressed to truly achieve sustainable, green implementation of these methods. We hope this review encourages a more critical perspective among readers and promotes the development of genuinely greener sample preparation strategies across different analytical applications.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 8","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-07-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148630795","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}
引用次数: 0
Direct Liquid Injection in Comprehensive Two-Dimensional Gas Chromatography Hyphenated to Quadrupole Time-of-Flight Mass Spectrometry Quality Profiling of Commercial Whiskies 双向气相色谱-四极杆飞行时间质谱联用直接进样法分析商业威士忌的质量。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-07-14 DOI: 10.1002/jssc.70490
Brian R. van 't Veer, Sander Affourtit, Hans-Gerd Janssen
{"title":"Direct Liquid Injection in Comprehensive Two-Dimensional Gas Chromatography Hyphenated to Quadrupole Time-of-Flight Mass Spectrometry Quality Profiling of Commercial Whiskies","authors":"Brian R. van 't Veer,&nbsp;Sander Affourtit,&nbsp;Hans-Gerd Janssen","doi":"10.1002/jssc.70490","DOIUrl":"10.1002/jssc.70490","url":null,"abstract":"<p>Luxury food products such as olive oil, wine, and whisky are highly vulnerable to fraudulent practices. Their chemical complexity, fortunately, provides numerous potential adulteration markers, but unfortunately also necessitates the use of powerful, comprehensive profiling approaches involving detailed methods for sample cleanup and analysis. One technique capable of both targeted marker analysis and untargeted profiling is comprehensive two-dimensional gas chromatography coupled to high-resolution mass spectrometry (GC×GC-HRMS). However, as with other chromatographic methods, this technique typically requires substantial sample preparation to eliminate contaminants, which increases the risk of losing valuable information. To address this issue, a direct-injection GC×GC-HRMS technique was developed for comprehensive quality profiling of whiskies. Multiple injection parameters were optimized to deal with the direct injection of a large series of whiskies with a focus on data quality. Overall, carryover percentages of less than 1.5% were obtained, except for long-chain linear acids, sugar-related compounds, and lignin-related compounds (carryover at most 7.1%, 11.4%, and 18%, respectively). The method demonstrated adequate sensitivity to identify numerous quality marker compounds. The developed method was applied to 59 whiskies, with some samples being measured in multiple sequences to assess method stability. Finally, chemometric analyses proved the data to be of good quality. By employing techniques such as principal component analysis, hierarchical clustering analysis, and partial least squares regression, valuable information was obtained, including insights into the preparation process and prize categorization.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 7","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70490","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148437027","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}
引用次数: 0
A Quick and Simple Chromatographic Method to Investigate the Adsorption of Glufosinate on a Subtropical Oxisol: Affinity Comparisons With Glyphosate 一种快速简便的色谱法研究草甘膦在亚热带草甘膦上的吸附:与草甘膦的亲和性比较。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-07-14 DOI: 10.1002/jssc.70491
Tatiana Valeria Furquim, Luan Viana, Jorge C. Masini
{"title":"A Quick and Simple Chromatographic Method to Investigate the Adsorption of Glufosinate on a Subtropical Oxisol: Affinity Comparisons With Glyphosate","authors":"Tatiana Valeria Furquim,&nbsp;Luan Viana,&nbsp;Jorge C. Masini","doi":"10.1002/jssc.70491","DOIUrl":"10.1002/jssc.70491","url":null,"abstract":"<div>\u0000 \u0000 <p>This work presents a fast and straightforward chromatographic method with fluorescence detection to quantify glufosinate in soil solutions. The method is based on the reaction between the primary amine group of glufosinate and <i>o-</i>phthaldialdehyde with 2-mercaptoethanol, producing a stable fluorescent derivative in under 2 min, which remains stable for more than 70 min (relative standard deviation [RSD] = 3.6%). The method does not require automated timing systems. Glyphosate, which lacks a primary amine, does not interfere, and potential interferences from aminomethyl phosphonic acid and ammonium are effectively circumvented by chromatographic separation, as their indole derivatives are well resolved from the glufosinate derivative. An isocratic chromatographic run using 20:80 methanol:piperazine-<i>N</i>,<i>N</i>′-bis(2-ethanesulfonic acid) buffer at 1.0 mL/min lasts 5 min. The method showed linearity over the concentration range of 0.10 and 20 µmol/L, with detection and quantification limits of 0.015 and 0.050 µmol/L, respectively. Calibration curve reproducibility is high (slope RSD &lt; 2.1%, <i>n</i> = 5). The method was effectively applied to study glufosinate adsorption in an Oxisol, revealing a maximum adsorption capacity of 2.5 ± 0.2 µmol/g, significantly lower than that reported for glyphosate.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 7","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148437070","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}
引用次数: 0
Quantitative Profiling and Metabolic Study of Caffeoylquinic Acids and Their Metabolites by Liquid Chromatography-Tandem Mass Spectrometry in Rats and Laying Hens 大鼠和蛋鸡体内咖啡酰奎宁酸及其代谢产物的液相色谱-串联质谱定量分析与代谢研究。
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-07-10 DOI: 10.1002/jssc.70485
Sichao Wang, Wenjie Tian, Xiaohui Feng, Huiyan Zhang, Youyou Yang, Junmin Zhang
{"title":"Quantitative Profiling and Metabolic Study of Caffeoylquinic Acids and Their Metabolites by Liquid Chromatography-Tandem Mass Spectrometry in Rats and Laying Hens","authors":"Sichao Wang,&nbsp;Wenjie Tian,&nbsp;Xiaohui Feng,&nbsp;Huiyan Zhang,&nbsp;Youyou Yang,&nbsp;Junmin Zhang","doi":"10.1002/jssc.70485","DOIUrl":"10.1002/jssc.70485","url":null,"abstract":"<div>\u0000 \u0000 <p>Caffeoylquinic acids are natural polyphenolic compounds with notable antioxidant and anti-inflammatory activities. This study developed and validated a sensitive high-performance liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of isochlorogenic acid A (ICQA) and 22 metabolites in serum. The method exhibited excellent sensitivity with limits of quantification of 0.625–1.25 µg/L (signal-to-noise ratio = 10), inter/intra-day precision below 15%, and comprehensive coverage of phase I/II and microbial metabolites. Application of the method in rats and laying hens demonstrated its robustness for pharmacokinetic profiling and cross-species validation, revealing a triphasic metabolic pattern of ICQA, the consistent metabolic endpoints of the accumulation of microbial metabolites, and a critical role of gut microbiota in ICQA metabolism. The developed platform provides a reliable analytical tool for comprehensive metabolism studies of phenolic compounds, with high throughput and reproducibility.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 7","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148422123","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}
引用次数: 0
Systemic Exposure and Multicomponent Pharmacokinetics of Mailuoning Oral Liquid: Integrated Ultra-High-Performance Liquid Chromatography-High-Resolution Mass Spectrometry Profiling and Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry Quantification 脉络宁口服液的全身暴露及多组分药动学:超高效液相色谱-高分辨率质谱分析和超高效液相色谱-串联质谱定量
IF 3.6 3区 工程技术
Journal of separation science Pub Date : 2026-07-10 DOI: 10.1002/jssc.70481
Sijia Wu, Wangya Jia, Jiekai Hua, Jie Jian, Linyan Zhu, Sheyu Jiang, Aizhen Xiong, Jian Li, Lili Ji, Wei Liu, Hong Xu
{"title":"Systemic Exposure and Multicomponent Pharmacokinetics of Mailuoning Oral Liquid: Integrated Ultra-High-Performance Liquid Chromatography-High-Resolution Mass Spectrometry Profiling and Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry Quantification","authors":"Sijia Wu,&nbsp;Wangya Jia,&nbsp;Jiekai Hua,&nbsp;Jie Jian,&nbsp;Linyan Zhu,&nbsp;Sheyu Jiang,&nbsp;Aizhen Xiong,&nbsp;Jian Li,&nbsp;Lili Ji,&nbsp;Wei Liu,&nbsp;Hong Xu","doi":"10.1002/jssc.70481","DOIUrl":"10.1002/jssc.70481","url":null,"abstract":"<div>\u0000 \u0000 <p>Mailuoning oral liquid (MLN) is a state-approved multi-herb formula that has been prescribed for 25 years to clear heat, nourish yin, invigorate blood, and resolve stasis. Although randomized controlled trials and real-world evidence support its efficacy in thromboangiitis obliterans, deep-vein thrombosis, and the convalescent phase of cerebral infarction, a systematic search identified no pharmacokinetic data on its bioactive constituents. This lack of pharmacokinetic data impedes evidence-based dose refinement and international acceptance. Here, we employed ultra-high-performance liquid chromatography with Quadrupole-Exactive Orbitrap high-resolution mass spectrometry (UHPLC-Q-Exactive Orbitrap HRMS) to track 39 MLN-derived compounds in rat plasma, intestinal contents, and 10 tissues; 15 with prominent systemic exposure were designated as key pharmacokinetic markers. A selective and sensitive UHPLC-tandem MS assay was subsequently developed and fully validated for simultaneous quantification of these 15 circulating components. The assay exhibited excellent linearity (<i>r</i> ≥ 0.9974) for all analytes, with precision, accuracy, extraction recovery, and matrix effects meeting standard bioanalytical validation criteria. All compounds demonstrated stability under the tested storage conditions. Following oral administration of MLN at 8.1 and 16.2 mL·kg<sup>−1</sup> in rats, all 15 components were rapidly absorbed, reaching peak plasma concentrations within approximately 1 h. Systemic exposure increased in a clear dose-dependent manner, with structurally related compounds showing similar pharmacokinetic profiles. Notably, the iridoids secoxyloganin, harpagide, and secologanic acid yielded the highest AUC<sub>0</sub>–<sub>24 h</sub> values, indicating they are the principal systemic exposure markers. This study establishes the first comprehensive pharmacokinetic profile for MLN and provides a robust, validated analytical platform. By creating a crucial link between quantitative systemic exposure and efficacy, our work supplies a scientific foundation for refining dosage regimens, establishing quality specifications, and promoting the evidence-based clinical application of this widely prescribed traditional Chinese medicine formula.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 7","pages":""},"PeriodicalIF":3.6,"publicationDate":"2026-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148422146","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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