Journal of Chromatography A最新文献_第6页

Selective isolation of Artepillin C from Brazilian green propolis by countercurrent chromatography 用逆流色谱法从巴西绿蜂胶中选择性分离青蒿素 C

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-20 DOI: 10.1016/j.chroma.2025.465977

Cristiane Cardoso dos Santos , Alicia Fontoura da Silva , Rosane Nora Castro , Gilda Guimarães Leitão

{"title":"Selective isolation of Artepillin C from Brazilian green propolis by countercurrent chromatography","authors":"Cristiane Cardoso dos Santos , Alicia Fontoura da Silva , Rosane Nora Castro , Gilda Guimarães Leitão","doi":"10.1016/j.chroma.2025.465977","DOIUrl":"10.1016/j.chroma.2025.465977","url":null,"abstract":"<div><div>The selective isolation by countercurrent chromatography of artepillin C, a prenylated derivative of <em>p</em>-coumaric acid, directly from the ethanol extract of Brazilian green propolis in a single step was developed using a two-phase system containing organic solvent and a basic aqueous solution, based on the ionization ability of carboxyl groups in a basic medium, which allows the selective extraction of compounds such as artepillin C to the aqueous phase, in the form of a salt. The solvent system hexane - 5 % aqueous Na<sub>2</sub>CO<sub>3</sub> was first optimized with different proportions of ethyl acetate, with the hexane - ethyl acetate ratio 1:1 - 5 % aqueous Na<sub>2</sub>CO<sub>3</sub> being selected. Fractionation of the ethanol extract of green propolis with this solvent system yielded artepillin C with a purity of 72 %. However, the high pH obtained with the Na<sub>2</sub>CO<sub>3</sub> solution also ionized other acidic derivatives (triterpenic acids and other phenolic derivatives) and the base was replaced by 4 % NaHCO<sub>3</sub>. The composition of the organic phase was re-optimized, with a ratio of hexane - ethyl acetate (8:2) and 4 % aqueous NaHCO<sub>3</sub> (1:1, v/v). Fractionation of the ethanol extract of green propolis with this new optimized solvent system provided artepillin C with a purity of 81 %, ensuring an excellent separation from the other compounds in the extract. The lower basicity of the bicarbonate solution was not able to ionize other acidic compounds, and the lower concentration of ethyl acetate prevented the loading of salt into the organic phase.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465977"},"PeriodicalIF":3.8,"publicationDate":"2025-04-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143874590","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Effect of stationary phase surface chemistry and particle architecture in proteomics 固定相、表面化学和粒子结构在蛋白质组学中的作用

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-20 DOI: 10.1016/j.chroma.2025.465976

Jan Valášek, Lukáš Hekerle, Martina Nechvátalová, Antonín Bednařík, Jan Preisler, Jiří Urban

{"title":"Effect of stationary phase surface chemistry and particle architecture in proteomics","authors":"Jan Valášek, Lukáš Hekerle, Martina Nechvátalová, Antonín Bednařík, Jan Preisler, Jiří Urban","doi":"10.1016/j.chroma.2025.465976","DOIUrl":"10.1016/j.chroma.2025.465976","url":null,"abstract":"<div><div>The kinetic properties of four columns packed with fully porous particles and three with superficially porous particles were characterized for possible application in proteomic bottom-up analyses. All columns provided an attachment of hydrophobic C18 chains at the surface of the stationary phase. However, they differed in the additional attachment of polar groups and/or endcapping procedure. We have used the retention modeling protocol to explore the separation efficiency and maximal achievable peak capacity on tested columns. Almost all columns provided comparable maximal peak capacity in the range of 500 – 700 for the eight-hour gradient run. This confirms that the family of the stationary phases used in the bottom-up proteomics can be extended. In the case of fully porous particles, we found that the higher the column peak capacity, the higher the number of identified peptides in the simple proteomic sample, with approximately one identified peptide per peak capacity unit. On the contrary, in the case of the superficially porous particles, the number of identified peptides in the sample decreased with the higher column peak capacity. This trend can be overturned only when the lower amount of the sample is injected. Hence, when bottom-up proteomics is considered, the lower loadability of the superficially porous particles still needs to be addressed. Most stationary phases tested can be successfully used in the bottom-up analyses. However, the stationary phases with incorporated polar functional groups reduced the undesirable contribution of free silanol groups to peptide peak tailing and increased the information provided by LC-MS analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465976"},"PeriodicalIF":3.8,"publicationDate":"2025-04-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143877150","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Dimethyl carbonate as a green mobile phase modifier for reversed phase liquid chromatography of polar aromatic and polyaromatic hydrocarbons 绿色流动相改性剂碳酸二甲酯用于极性芳烃和多芳烃反相液相色谱

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-20 DOI: 10.1016/j.chroma.2025.465975

Philip D. Boes, Abdullah A. Alqahtani, Mohamed A. Abdelaziz, Neil D. Danielson

{"title":"Dimethyl carbonate as a green mobile phase modifier for reversed phase liquid chromatography of polar aromatic and polyaromatic hydrocarbons","authors":"Philip D. Boes, Abdullah A. Alqahtani, Mohamed A. Abdelaziz, Neil D. Danielson","doi":"10.1016/j.chroma.2025.465975","DOIUrl":"10.1016/j.chroma.2025.465975","url":null,"abstract":"<div><div>Linear alkyl carbonate solvents such as dimethyl carbonate (DMC) are considered to be environmentally safe with a low toxicology risk. The modest viscosity of 0.625 mPa·s and the UV cutoff wavelength of about 215 nm makes DMC a potential alternative aprotic HPLC modifier solvent to acetonitrile. The main issue is the limited solubility of DMC in water, about 14 %. A polarity parameter (P’) for DMC of 3.4 ± 0.1 was determined by ratioing Hildebrand solubility parameters for three alcohols and DMC to the corresponding alcohol P’ values. A test mixture of polar aromatic compounds (benzene sulfonate, aminobenzoic acid, nitrobenzoic acid, salicylic acid, and <em>N,N</em>-dimethylaminobenzoic acid) has a reasonable retention factor (<em>k</em>) range between 1 and 9 over a DMC modifier percentage of 10 to 2 % with no ethanol as the co-solvent using a C-18 column. For a similar retention factor range using methanol, the composition required variation from 60 to 10 %. Compatibility of DMC with the ion pairing agent tetrabutylammonium has been shown, increasing the retention of benzene sulfonate and lowering the retention of the aminobenzoic acids. Average solvent strength parameters calculated from quadratic fits of ln <em>k</em> versus organic mobile phase fraction for caffeine, sulfathiazole, and two nitroaniline isomers have shown DMC to be significantly higher (2.8) than ethanol (1.7) or acetonitrile 1.6). This water solubility limitation of DMC can be overcome by using ethanol as a co-solvent, still maintaining the green nature of the mobile phase, at a 5:3 DMC:ethanol ratio. DMC has proven to be an effective RPLC modifier solvent, with either UV or fluorescence detection, for hydrophobic polyaromatic hydrocarbons (PAHs) such as the seven ring coronene, reducing its retention by a factor of 5 as compared to acetonitrile.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465975"},"PeriodicalIF":3.8,"publicationDate":"2025-04-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143892176","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Mitigating the effects of organic solvents in sample diluents for ion chromatography: A comprehensive study and guidelines for optimization 减轻离子色谱样品稀释剂中有机溶剂的影响：一项全面的研究和优化指南

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-19 DOI: 10.1016/j.chroma.2025.465974

Mingwan Leng , Frank Bernardoni , Heather Wang , Sachin Lohani , Erik L. Regalado , Christopher A Pohl , Tianyu Yuan

{"title":"Mitigating the effects of organic solvents in sample diluents for ion chromatography: A comprehensive study and guidelines for optimization","authors":"Mingwan Leng , Frank Bernardoni , Heather Wang , Sachin Lohani , Erik L. Regalado , Christopher A Pohl , Tianyu Yuan","doi":"10.1016/j.chroma.2025.465974","DOIUrl":"10.1016/j.chroma.2025.465974","url":null,"abstract":"<div><div>Ion Chromatography (IC), the gold standard for the separation and analysis of ionic species, has been extensively used for detection of ions in industrial applications. Pharmaceutical samples with limited water solubility often require the use of organic solvents as diluents, which can pose significant challenges on IC analysis. Herein, the effects of various organic solvents as sample diluents in IC for anion analysis are systematically investigated. Electrochemically stable solvents such as 2-propanol (IPA), acetone, and dimethyl sulfoxide (DMSO) were found to have the least impact on the IC baseline. For solvents with a greater impact, a solvent dilution device (SDD) has been designed to minimize their effects. The device effectively diluted the organic solvents before they reached the suppressor electrode, reducing the generation of oxidized products. The results showed that the baseline stability and separation efficiency of IC can be maintained when using a wide range of organic solvents as diluents. Notably, the use of a solvent dilution device enabled good recovery of ions in various active pharmaceutical ingredients and significantly enhanced the signal to noise ratio of early-eluting ions compared to analyses conducted without the device. Guidelines are proposed to minimize the impact of organic solvents in IC sample preparation and anion analysis. The study also investigates the origin of impurity peaks introduced by the organic solvents and demonstrated the effectiveness of an ion-exchange resin treatment for their removal. Overall, this study provides insights for the use of organic solvents as IC diluents and offers practical solutions to overcome their challenges in pharmaceutical applications.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465974"},"PeriodicalIF":3.8,"publicationDate":"2025-04-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143874511","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Chemical safety screening of products – better proactive 产品的化学安全筛选-更积极主动

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-19 DOI: 10.1016/j.chroma.2025.465946

Gertrud E. Morlock

{"title":"Chemical safety screening of products – better proactive","authors":"Gertrud E. Morlock","doi":"10.1016/j.chroma.2025.465946","DOIUrl":"10.1016/j.chroma.2025.465946","url":null,"abstract":"<div><div>The increasing pressure to ensure product safety in a global market comes up against the current practice of targeting only known hazardous compounds in product safety analysis. However, product safety refers not only to known but also to unknown or hidden hazards that are very important to know and avoid. Shortcomings and limitations of currently used technologies seem to cause an obvious discrepancy between intended and actual consumer protection. Products are not as safe as claimed by stakeholders. An existing but overlooked proactive safety screening with a prioritization strategy is brought into focus as it offers a unique solution. It can handle the complexity of a product with thousands of compounds of unknown identity and unknown toxicity and can figure out the important hazardous compounds, both known and unknown. Using hardly any sample preparation and the effect detection at an early position in the workflow is a game changer not to overlook hazardous compounds. All analytical technologies are needed, but the key is the re-arrangement of the instrument order, <em>i.e.</em> firstly hazard-related screening (effect first) and secondly, focus on identification of prioritized hazardous compounds. Such a proactive safety screening revealed previously unknown hazardous compounds in products on the market claimed to be safe. The highly sustainable, affordable, and all-in-one 2LabsToGo-Eco with easy-to-use planar bioassays empowers stakeholders to implement proactive safety screening and dynamic risk management. The transition to greater efficacy in consumer protection needs incentives and the critical review aims to stimulate a debate.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465946"},"PeriodicalIF":3.8,"publicationDate":"2025-04-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143848610","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Insight into photocatalyzed transformations of multiclass organic contaminants in water 洞察光催化转化多类有机污染物在水中

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-16 DOI: 10.1016/j.chroma.2025.465971

Aleksander Kravos , Federico Cristaudo , Federica Dal Bello , Claudio Medana , Helena Prosen , Paola Calza

{"title":"Insight into photocatalyzed transformations of multiclass organic contaminants in water","authors":"Aleksander Kravos , Federico Cristaudo , Federica Dal Bello , Claudio Medana , Helena Prosen , Paola Calza","doi":"10.1016/j.chroma.2025.465971","DOIUrl":"10.1016/j.chroma.2025.465971","url":null,"abstract":"<div><div>This study investigates three understudied emerging contaminants: pharmaceutical ramipril (RAM), artificial sweetener neotame (NEO), and herbicide cycloxydim (CYC). Laboratory simulations of natural photoinduced transformations were conducted exploring direct photolysis and TiO<sub>2</sub> photocatalysed process, followed by analysis with tandem high-resolution mass spectrometry (HRMS). The contaminants exhibited low-to-medium degree of photolysis, but rapid dissipation under photocatalysis. The assessment of transformation products (TPs) revealed several analytical challenges, particularly in peak detection and data management. The structural elucidation of the abundant TPs was achieved through multi-stage MS fragmentation studies and the transformation pathways were proposed based on the identified structures, evolution profiles, and polarities. The hydroxylation was the most common transformation for all contaminants, although each showed unique additional pathways. For instance, RAM underwent intermolecular cyclization, forming a diketopiperazine-like TP, as well as ketone formation and cleavage into low molecular mass TPs. NEO experienced ester hydrolysis, reduction, resulting in C=C bond formation, and oxidative aromatic ring-opening reactions. Lastly, CYC displayed (poly)hydroxylation or transformations of its oxime ether moiety, which underwent hydrolysis, detachment, or rearrangement, leading to oxazole TPs. The ECOSAR software was used for the prediction of toxicities of the identified TPs. <em>In-silico</em> toxicity prediction showed that the hydroxylated phenolic TPs of NEO and RAM, as well as certain oxazole TP isomers of CYC, have the potential to increase overall toxicity during the degradation. Overall, this paper addresses the analytical challenges and innovative methodologies for studying TPs, highlighting their growing relevance in environmental analytical chemistry.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465971"},"PeriodicalIF":3.8,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143864594","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Cationic conjugated microporous polymers for efficient quinolone antibiotics extraction: Experimental and DFT study 阳离子共轭微孔聚合物用于喹诺酮类抗生素的高效提取：实验和DFT研究

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-16 DOI: 10.1016/j.chroma.2025.465973

Gui-Cheng Ge , Na Li , Ying-Jie Hao , Ling-Xi Zhao , Xiaoli Wang , Lu Liu , Xiangfeng Chen , Houmei Liu , Yaqi Cai , Ru-Song Zhao

{"title":"Cationic conjugated microporous polymers for efficient quinolone antibiotics extraction: Experimental and DFT study","authors":"Gui-Cheng Ge , Na Li , Ying-Jie Hao , Ling-Xi Zhao , Xiaoli Wang , Lu Liu , Xiangfeng Chen , Houmei Liu , Yaqi Cai , Ru-Song Zhao","doi":"10.1016/j.chroma.2025.465973","DOIUrl":"10.1016/j.chroma.2025.465973","url":null,"abstract":"<div><div>The development of exquisitely sensitive analytical methods for the surveillance of quinolone antibiotics (QAs) holds pivotal significance in safeguarding both ecosystems and human well-being. In this work, a cationic conjugated microporous polymer (iCMP) was constructed through a facile post-synthetic approach. Capitalizing on its unique dual-porosity architecture, cationic framework, and π-conjugated backbone, iCMP exhibited exceptional adsorption capabilities and remarkable repeatability. Integrating with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), a solid-phase extraction (SPE) method founded on iCMP was meticulously developed for the sensitive and accurate detection of QAs within complex matrices. This proposed analytical method exhibited remarkably low limits of detection, specifically 0.0200–0.128 ng·L<sup>-1</sup> for water samples and 0.0250–0.105 ng·g<sup>-1</sup> for meat samples, along with good accuracy in the range of 70.9 %-115 %. The underlying adsorption mechanism was comprehensively investigated using a synergistic approach that combined systematic adsorption experiments, density functional theory (DFT) calculations, and in-depth material characterizations. Overall, this study presents viable strategies for the precise trace-level analysis of QAs in complex environmental and food samples.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465973"},"PeriodicalIF":3.8,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143855527","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Systematic comparison of wide pore size exclusion chromatography columns for the characterization of gene therapy products 大孔径排阻色谱柱用于基因治疗产品表征的系统比较

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-16 DOI: 10.1016/j.chroma.2025.465972

Mathias Buff , Alexandre Goyon , Carsten Elger , Raphael Ruppert , Markus Haindl , Kelly Zhang , Davy Guillarme

{"title":"Systematic comparison of wide pore size exclusion chromatography columns for the characterization of gene therapy products","authors":"Mathias Buff , Alexandre Goyon , Carsten Elger , Raphael Ruppert , Markus Haindl , Kelly Zhang , Davy Guillarme","doi":"10.1016/j.chroma.2025.465972","DOIUrl":"10.1016/j.chroma.2025.465972","url":null,"abstract":"<div><div>A new generation of wide pore SEC columns was systematically evaluated for the determination of size variants for mRNAs ranging from 1000 to 5000 nucleotides and for multiple recombinant adeno-associated viruses (rAAVs) serotypes. Among the six SEC columns (450 to 700 Å) employed for rAAV analysis, the DNACore AAV-<em>SEC</em> column shows the highest efficiency (11,000 plates), probably due to its monodisperse 3 µm silica particles, while the SRT SEC-500 column showed the lowest efficiency (< 1000 plates) attributed to its 5 µm particle packing. Optimal selectivity for rAAVs was observed with columns having larger pore sizes (550 - 700 Å). However, the final resolution for different rAAV serotypes was highly sample-dependent, and no single column consistently provided the best separation of size variants. Additionally, the six columns were suitable to study the degradation trends of rAAVs subjected to accelerated stress conditions. Among the five SEC columns (700 - 1000 Å) evaluated for mRNA analysis, the Biozen dSEC-7 LC column (700 Å) column systematically achieved the highest efficiency, and was particularly well suited for analyzing small mRNA (∼ 1000 nts). However, columns with larger pore sizes such as AdvanceBio SEC 1000A were more appropriate for larger mRNA (> 1000 nt). Despite these findings, the separation of low molecular weight species (LMWS) and high molecular weight species (HMWS) of mRNA remains limited across all tested columns, making integration challenging and the quantification of LMWS and HMWS less accurate. However, comparable (but not strictly identical) quantitative performance was obtained among the columns, with only a few exceptions.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465972"},"PeriodicalIF":3.8,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143864593","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Development of a magnetic beads-based ligand fishing method for screening SARS-CoV-2 NSP5 inhibitors from complex herbal mixtures: Rosmarinus officinalis as a case study 基于磁珠的配体捕捞方法在复杂草药混合物中筛选SARS-CoV-2 NSP5抑制剂：以迷迭香为例

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-16 DOI: 10.1016/j.chroma.2025.465956

Yujing Huang , Duntao Zu , Chenjing Tian , Juntao Xie , Wenlin Chen , Hongxia Fan , Xin Yu , Huiqing Lu , Jianni Yang , Fulong Lin , Junxia Zheng

{"title":"Development of a magnetic beads-based ligand fishing method for screening SARS-CoV-2 NSP5 inhibitors from complex herbal mixtures: Rosmarinus officinalis as a case study","authors":"Yujing Huang , Duntao Zu , Chenjing Tian , Juntao Xie , Wenlin Chen , Hongxia Fan , Xin Yu , Huiqing Lu , Jianni Yang , Fulong Lin , Junxia Zheng","doi":"10.1016/j.chroma.2025.465956","DOIUrl":"10.1016/j.chroma.2025.465956","url":null,"abstract":"<div><div>SARS-CoV-2 NSP5, a conserved protease essential for viral replication, represents a critical therapeutic target. Natural products provide diverse chemical scaffolds for antiviral development but remain underexploited. Traditional screening methods struggle to resolve specific inhibitors in complex herbal matrices due to selectivity and throughput limitations. To address these challenges, we developed an innovative magnetic beads-based ligand fishing strategy coupled with UPLC-Q-Exactive-Orbitrap-MS/MS for rapid discovery of SARS-CoV-2 NSP5 inhibitors from complex herbal matrices. Screening of 44 traditional Chinese medicinal extracts identified <em>Rosmarinus officinalis</em> as a potent inhibitor, exhibiting an IC<sub>50</sub> of 19.90 ± 3.16 μg/mL against NSP5. Through ligand fishing and mass spectrometry analysis, 15 bioactive compounds were identified, including 8 diterpenoids (predominantly abietane-type) and 3 phenylpropanoids. Notably, rosmarinic acid demonstrated the strongest inhibition (IC<sub>50</sub> = 5.784 ± 0.20 μM), surpassing the positive control ebselen in molecular docking studies. Structural characterization revealed that hydroxyl and carboxyl groups in diterpenoids formed critical hydrogen bonds with catalytic residues (Cys145, Ser144) of NSP5. This methodological advancement not only improved the accuracy of natural product screening but also facilitated the development of targeted antiviral strategies against SARS-CoV-2 and other emerging viral pathogens.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465956"},"PeriodicalIF":3.8,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143879130","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Integration of HPTLC with ATR-FTIR, HRMS and bioquantification for evaluation of antibacterial and antioxidant compounds in marine sponges HPTLC与ATR-FTIR、HRMS和生物定量相结合评价海绵中抗菌和抗氧化成分

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-04-14 DOI: 10.1016/j.chroma.2025.465967

Miljan Bigović , Marko Jović , Marko Nikolić , Slavica Petović , Petar Ristivojević

{"title":"Integration of HPTLC with ATR-FTIR, HRMS and bioquantification for evaluation of antibacterial and antioxidant compounds in marine sponges","authors":"Miljan Bigović , Marko Jović , Marko Nikolić , Slavica Petović , Petar Ristivojević","doi":"10.1016/j.chroma.2025.465967","DOIUrl":"10.1016/j.chroma.2025.465967","url":null,"abstract":"<div><div>Marine sponges are an abundant source of unique bioactive compounds, offering immense potential for the development of innovative medicines. This study presents an analytical approach for the identification of bioactive compounds in marine sponge extracts. The approach capitalizes high-performance thin-layer chromatography (HPTLC) - Effect-Directed Analysis (EDA) with high-resolution mass spectrometry (MS) and Fourier-transform infrared (FTIR) spectroscopy, enabling identification of bioactive compounds. HPTLC-EDA was done to evaluate radical scavenging and antimicrobial activities against five pathogenic bacterial strains<em>: Escherichia coli, Klebsiella pneumoniae, Bacillus spizizenii, Staphylococcus aureus,</em> and methicillin-resistant <em>Staphylococcus aureus</em> (MRSA). The bioquantification of streptomycin and gallic acid was conducted using image analysis of HPTLC chromatograms, with subsequent analysis via antimicrobial assays against the aforementioned bacterial strains and DPPH (2,2-diphenyl-1-picrylhydrazyl) radical scavenging assays. The developed HPTLC chromatograms, utilizing toluene:ethyl acetate:acetic acid (60:37.5:2.5, <em>V</em>/<em>V</em>/<em>V</em>) as a mobile phase for the first time, enabled the optimal separation of bioactive compounds from complex marine sponge extracts. Avarol from <em>Dysidea avara</em> was identified as the compound with the highest potential using FTIR and HRMS techniques. The study highlights a high-throughput, cost-effective approach for screening bioactive metabolites from marine sponges using HPTLC-bioassay. This approach accelerates therapeutic discovery and offers a sustainable, eco-friendly alternative to traditional methods.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1752 ","pages":"Article 465967"},"PeriodicalIF":3.8,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143850512","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0