TALANTA
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2022
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IF 6.556
Yang Xu,Yanfang Liu,Han Zhou,Rong Wang,Dongping Yu,Zhimou Guo,Xinmiao Liang
Natural products , especially alkaloids, are one of the most valuable, potential drug leads in drug discovery. As an efficient tool for complex samples, two-dimensional liquid chromatography (2D-LC) has become a powerful means of analysis and separation of natural alkaloids. Method development of 2D-LC is of great importance because it helps to enhance the selectivity, resolution and peak capacity of a separation system. However, due to the diversity of the nature and subclasses of natural alkaloids, peak tailing occurs frequently, making alkaloid separation complicated and time-consuming. To conquer such difficulties, we proposed a guide for column selection and combination in 2D-LC so as to improve the alkaloid separation. Based on a comprehensive evaluation of applicability and orthogonality of several columns, this guide would provide a simple but clear starting point for column selection of 2D-LC method development. The evaluation included seven columns to involve most separation mechanisms reported in alkaloid separation, and 49 natural alkaloid standards of various subclasses and natures. Detailed studies of peak shapes of every column were carried out as well, providing useful references to better understand the peak tailing issues of some analytes on specific columns. Subsequently, a 2D-LC method was developed using our guide to isolate an alkaloid sample from U. rhynchophylla , generating symmetrical peaks and a high orthogonality of 80.3%. Further, this evaluation process would help to have a quick understanding when a new stationary phase is designed.
研究领域:
分析化学
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药学
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天然产物化学
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DOI
PubMed
高影响因子
MOLECULES
·
2024
·Vol. 29
·期 13
·3133
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IF 4.2
Qimei Wu,Jinfen Zheng,Yan Yu,Zhirong Li,Ying Li,Chengfeng Hu,Yaping Zhou,Rongxiang Chen
Vitex negundohas strong antioxidant activity, but its primary antioxidant components are not clear. In this study, the antioxidant components were screened by offline two-dimensional liquid chromatography coupled with electrochemical detection (2D-LC-ECD) and subsequently assessed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) identification, radical scavenging capacity, and molecular docking. Various fractions were isolated fromVitex negundoleaves, and 39 antioxidant components were screened and identified. All of the fractions containing the antioxidant components exhibited certain antioxidant activity. Correlation analysis revealed a strong correlation between the response of LC-ECD and the in vitro antioxidant activity of the fractions. Molecular docking demonstrated that components with high response to LC-ECD exhibited robust interaction with antioxidant-related target proteins. The main antioxidant components ofVitex negundoleaves were isoorientin, chlorogenic acid, agnuside, cynaroside, and scutellarin. The 2D-LC-ECD combined with LC-MS/MS was rapid and effective in screening the antioxidant components inVitex negundoleaves and could also provide technical support for the discovery of antioxidant components with different polarities and contents in other medicinal and edible plants.
研究领域:
植物化学
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分析化学
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药理学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2026
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IF 10.4
Xinrui Yang,Xiaoling Chen,Gaohan Li,Yang Zhou,Qinhua Chen,Jinjun Hou,Changwu Zheng,Zijia Zhang,Wanying Wu
Areca nut ( Areca catechu L.) is a widely consumed food and medicinal plant with both nutritional value and documented health risks. To comprehensively characterize its chemical composition and spatial distribution, we developed an integrated analytical platform combining solid-phase extraction (SPE), offline two-dimensional liquid chromatography with high-resolution mass spectrometry (2D-LC-HRMS), and desorption electrospray ionization mass spectrometry imaging (DESI-MSI). This approach enriched trace constituents while minimizing matrix interference, enabling the identification of 323 compounds-including terpenes and triterpenoids (89), alkaloids (52), flavonoids (31), lignans (17), and steroids (12). A pH-orthogonal separation system (alkaline and acidic modes) significantly improved resolution of structurally similar, low-abundance compounds. Spatial analysis via DESI-MSI revealed three distribution patterns: seed-specific enrichment, pericarp enrichment, and uniform distribution. By integrating compositional and spatial data, this study offers new insights into the pharmacological basis, potential toxicity mechanisms, and safe applications of areca nut in food systems.
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高影响因子
ANALYTICA CHIMICA ACTA
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2025
·
IF 6
Shiwen Zhou,He Tang,Lu Gao,Wangyu Li,Jiancong Liao,Xihe Yang,Yuanjiang Pan,Hongru Feng
Background Oligonucleotide-based drugs have gained significant attention as a promising class of therapeutics due to their precise ability to regulate gene expression. However, the presence of impurities in these drugs can compromise their safety, efficacy, and stability. Therefore, the identification and detailed analysis of these impurities are crucial. Traditional methods may struggle to detect subtle impurities, such as oxidation and hydrolysis products, which necessitate the development of more advanced and reliable analytical techniques for oligonucleotide therapeutics. Results In this study, we introduce a novel analytical method that combines heart-cutting two-dimensional liquid chromatography (2D-LC) with tandem mass spectrometry (MS/MS) to effectively separate, analyze, and identify impurities in oligonucleotide-based drugs. The first dimension utilizes anion exchange chromatography (AEX) to separate oligonucleotides based on their negative charge, while the second dimension employs reverse ion-pair chromatography (RIPC) for further purification and compatibility with mass spectrometry. This 2D-LC-MS/MS approach provides a sensitive and accurate means of identifying and quantifying impurities, including oxidation and hydrolysis products. The method was applied to two RNA interference (RNAi) drugs, Givosiran and Patisiran, where 3 and 20 impurities were identified, respectively. Additionally, sequencing analysis using data-dependent acquisition (DDA-MS/MS) enabled the determination of the molecular weight and structural characteristics of these impurities, offering a comprehensive and detailed view of the impurity profiles. Significance This novel heart-cutting 2D-LC-MS/MS method offers a significant advancement in the analysis of impurities in oligonucleotide-based therapeutics. It provides high sensitivity, enabling the identification of subtle impurities that are often challenging to detect. By applying this technique to RNAi drugs, we demonstrate its potential to enhance the safety, efficacy, and stability of oligonucleotide-based therapies, making it a valuable tool for the pharmaceutical industry.
研究领域:
药物分析
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分析化学
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生物治疗学
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质谱分析
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色谱分析
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药物研发
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生物药剂学
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PubMed
高影响因子
Antioxidants
·
2026
·Vol. 15
·期 8
·1008
·
IF 8.2
Zhengyan Tan,Pei Xu,Dan Wang,Zongna Han,Huaying Chen,Qianqian Zhu,Yang Yang,Wei Pan,Piao Wang,Rongxiang Chen
This study established an activity-oriented analysis method based on offline two-dimensional liquid chromatography–electrochemical detection (2D-LC-ECD) combined with ultra-high-performance liquid chromatography–Orbitrap-MS/MS (UHPLC-Orbitrap-MS/MS), which was used to comprehensively characterize the antioxidant components ofPolygonum multiflorumThunb. leaves (PML) and screen for differential compounds in samples from different origins. Antioxidant components were screened using 2D-LC-ECD combined with in vitro radical scavenging experiments; structure identification was conducted via UHPLC-Orbitrap-MS/MS, and chemometric analysis alongside quantitative determination of 19 major components was carried out across 31 batches of samples. A total of 43 potential antioxidant compounds were identified from PML, including 11 phenolic acids, 29 flavonoids, 2 stilbene glycosides, and 1 amino acid; phenolic acids and their derivatives, along with flavonoids, were identified as major contributors to antioxidant activity. Hierarchical clustering analysis and principal component analysis both grouped samples into four categories by origin; the orthogonal partial least squares discriminant analysis model (R2X = 0.933, R2Y = 0.941, Q2= 0.846) screened 10 key markers (VIP > 1). The quantitative results showed that polygonacetophenoside had the highest content in PML. In summary, the 2D-LC-ECD coupled with LC-Orbitrap-MS/MS strategy confirmed that phenolic acids and flavonoids are the core material basis for PML’s antioxidant capacity, providing scientific evidence for the industrial development of PML as a natural antioxidant.
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高影响因子
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