Rapid Communications in Mass Spectrometry最新文献

{"title":"A Robust and Accurate Filter Paper–Based Dried Plasma Spot Method for Bictegravir Monitoring in HIV Therapy","authors":"Arpita Sathyanarayanan,&nbsp;Roopashri N. Arekal,&nbsp;Divyashree Somashekara","doi":"10.1002/rcm.10110","DOIUrl":"https://doi.org/10.1002/rcm.10110","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Context</h3>\u0000 \u0000 <p>Therapeutic drug monitoring (TDM) involves the collection of biological samples such as blood, plasma, urine, and saliva. The most commonly used biological matrix for the detection of drugs is either blood or plasma, as they are widely accepted by the regulatory authorities. Such studies require a significant amount of blood to be collected and even more if the study is performed in a plasma sample. The growing demand to minimize the blood or biological samples required for the study of drugs, dried blood spot, or the dried plasma spot techniques has been studied by its demand.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Objective</h3>\u0000 \u0000 <p>The main aim was the development of a novel method for the determination of the circulating blood plasma levels in clinical samples using spotted and dried plasma on filter paper as a substrate detection of bictegravir, an HIV integrase strand transfer inhibitor (INSTI) drug from dried plasma spots.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Materials and Methods</h3>\u0000 \u0000 <p>The quantitation, as well as the detection of the plasma drug concentration, was done using liquid chromatography–tandem mass spectrometry LC-MS/MS. Sixty microliters of plasma spiked with 2% of the drug was spotted on Whatman filter paper and was left to dry at room temperature. The drug was extracted using methanol as a precipitating agent.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The extraction technique yielded a recovery of 100%. The assay exhibited excellent linearity in the range of 20–1200 ng/mL.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Discussion and Conclusion</h3>\u0000 \u0000 <p>The method developed is a robust, simple, and accurate method to extract drug from the plasma. This method enables to produce a clean sample, proving to be cheaper and more accurate with maximum recovery.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 21","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10110","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144705525","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Blood Collection Tube has Minimal Interference on the Carbon and Nitrogen Isotope Composition of Plasma, Red Blood Cells, and Serum in Cow Blood","authors":"David M. Jaramillo,&nbsp;Lisa M. Bauman,&nbsp;Carlos Henrique Paiva Camisa Nova,&nbsp;Lais Lima,&nbsp;Edzard van Santen","doi":"10.1002/rcm.10109","DOIUrl":"https://doi.org/10.1002/rcm.10109","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Stable isotopes can be useful for tracking diet composition and other physiological processes in ruminants. These techniques rely on the fact that tissues directly reflect the animal's diet. Blood is a dynamic tissue that can be separated into serum, plasma, and red blood cell (RBC) components. Numerous collection tubes for blood are commercially available. No studies have compared the isotopic composition from cattle blood as affected by collection tube. This study compared commercially available serum and plasma tubes and evaluated how they may affect δ¹³C, δ¹⁵N, and C and N concentrations from blood in lactating dairy cattle.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>For plasma and RBC, treatments were five collection tubes containing different anticoagulants: dipotassium ethylenediaminetetraacetic acid (K2EDTA), tripotassium EDTA (K3EDTA), NaF/K oxalate, Li heparin (LiHep), and Na heparin (NaHep). For serum analysis, the three collection tubes were a RedTop (contained no coagulating agent) and TigerTop and Red+CAT, which both contained clot activator and serum separator gel, each made by two different manufacturers. All samples were collected via tail venipuncture in cows. All samples were processed, freeze dried, and analyzed in triplicate for δ¹³C, δ¹⁵N, and C and N.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>While mean differences exist on the δ¹³C and δ¹⁵N from plasma and red blood cells, differences were minimal. Clot activator gels in serum tubes did not affect the δ¹³C and δ¹⁵N composition. This study showed that, while isotopic values may differ slightly from different blood collection tubes, these differences were often small, which may have little impact on the interpretation of research results when serum or RBC are analyzed. The isotopic composition of C and N concentrations of serum was not affected by the three tubes used within this study. Researchers will have to understand these differences and decide whether or not these may impact the objectives and the results of a given study.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 21","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144688143","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Acid Fractionation Factor of Oxygen Isotopes in Mixed Calcite–Dolomite Samples: Implications for Data Correction","authors":"Linlin Cui,&nbsp;Xu Wang,&nbsp;Lianjun Feng,&nbsp;Xiaomei Zhang","doi":"10.1002/rcm.10108","DOIUrl":"https://doi.org/10.1002/rcm.10108","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>The conventional method for measuring carbon and oxygen isotopes in carbonates involves the reaction of carbonate minerals with phosphoric acid (PPA) to generate CO₂, followed by purification and isotopic analysis. During this reaction, a temperature-dependent oxygen isotope acid fractionation factor (AFF) is introduced, as not all oxygen is released in CO₂. Although the temperature dependence of AFF has been extensively studied in pure carbonate minerals, little research has been conducted on AFF variations in mixed carbonate minerals with diverse chemical and mineralogical compositions. This study aims to investigate the range of AFF variations in carbonates containing multiple mineral phases.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Oxygen isotope compositions of CO₂ produced from CaCO₃-MgCO₃ mixed minerals reacting with PPA at 25°C, 50°C, 70°C, and 90°C were analyzed using a GasBench II system coupled with a Thermo Finnigan Delta V Plus isotope ratio mass spectrometer.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The AFF values for CaCO₃-MgCO₃ mixed minerals fall between those of pure calcite and dolomite, generally aligning with theoretical predictions. Additionally, the fractionation gradient (dδ¹⁸O/dT⁻¹) increases with rising mole Mg and dolomite content, indicating a systematic trend in fractionation behavior.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>These findings provide a framework for AFF correction based on mole Mg or dolomite content, enhancing the reliability and precision of oxygen isotope measurements in natural impure carbonates.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 21","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144672714","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Characterization of N-Terminal Acetylated α-Hemoglobin Stabilizing Protein (AHSP) by Top-Down High-Resolution Mass Spectrometry From Human Preterm Newborns Oral Fluid","authors":"Federica Iavarone,&nbsp;Chiara Tirone,&nbsp;Simona Fattore,&nbsp;Davide De Tomaso,&nbsp;Nicoletta Menzella,&nbsp;Giovanni Vento,&nbsp;Alessandra Olianas,&nbsp;Barbara Manconi,&nbsp;Tiziana Cabras,&nbsp;Giulia Guadalupi,&nbsp;Cristina Contini,&nbsp;Mozhgan Boroumand,&nbsp;Claudia Desiderio,&nbsp;Alexandra Muntiu,&nbsp;Antonella Fiorita,&nbsp;Matteo Fraschini,&nbsp;Vassilios Fanos,&nbsp;Gavino Faa,&nbsp;Irene Messana,&nbsp;Massimo Castagnola","doi":"10.1002/rcm.10107","DOIUrl":"https://doi.org/10.1002/rcm.10107","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Alpha-hemoglobin stabilizing protein (AHSP) is an erythroid-specific protein forming a stable complex with free α-hemoglobin, but not with β-hemoglobin or hemoglobin A (α₂β₂), thus preventing harmful aggregation of α-hemoglobin during normal erythroid cell development and avoiding its pro-oxidant activity. Although its function has been extensively studied in erythroid cells, its presence in preterm newborns' oral fluid remains unexplored. Given the high susceptibility of preterm infants to hematological disorders, characterizing AHSP in their oral fluid could provide valuable insights into fetal erythropoiesis and its potential role as a biomarker for neonatal anemia and transfusion needs.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>The primary structure of AHSP was determined by high-resolution top-down proteomic analysis using a nano-HPLC–ESI–MS/MS approach on oral fluid samples from preterm newborns. Specimens were collected non-invasively from infants, promptly treated with formic acid, and analyzed with an Orbitrap-based mass spectrometry platform. The intact protein's molecular mass and fragmentation pattern were assessed to determine its primary structure and post-translational modifications. Statistical analysis was performed to explore correlations between AHSP presence and neonatal clinical parameters, including anemia and transfusion needs.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The experimental monoisotopic molecular mass value [M + H⁺]¹⁺ at <i>m/z</i> 11744.958 ± 0.3 was inconsistent with the protein sequence reported in the literature, and the MS/MS fragmentation pattern was in agreement with the loss of the N-terminal methionine residue followed by Nα-terminal acetylation, a very common post-translational modification, now recognized as having an important role in modulating protein function, localization and protein stability and turnover. The sporadic samples having detectable amounts of AHSP resulted from preterm newborns with severe anemic status, while all were submitted to iron supplementation.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Although the data obtained so far cannot be used for quantitative analysis or statistical evaluation, AHSP appears to stand out as a potential early biomarker of neonatal hematological disorders, highlighting a new perspective for future investigations.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 21","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10107","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647260","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Deciphering Branched Galactomannan Structures via Multistage Ion Mobility MS and MSⁿ Fragmentation (Multistage IMSⁿ).","authors":"Rania Benazza, Mathieu Fanuel, Hélène Rogniaux, David Ropartz","doi":"10.1002/rcm.10100","DOIUrl":"https://doi.org/10.1002/rcm.10100","url":null,"abstract":"<p><strong>Rationale: </strong>Hemicelluloses are abundant carbohydrate components in plant cell walls. They play a crucial structural role in binding cellulose microfibrils, in addition to other biological functions. Their high structural variability directly influences their biological properties, making it important to establish a structure-function relationship. In the case of galactomannans, this complexity lies in branching, large size, in addition to isomerism, which makes their characterization challenging. In this context, we have demonstrated that cyclic ion mobility spectrometry (IMS), combined with porous graphitic carbon (PGC) chromatography, mass spectrometry (MS), and multistage MS/MS fragmentation (IMSⁿ), is a powerful tool for the detailed elucidation of galactomannan structures.</p><p><strong>Methods: </strong>In this study, we show that our multistage IMSⁿ sequencing approach, previously validated for homo-linear oligosaccharides (OS), can be successfully applied to hetero-branched hemicelluloses with careful adjustments. Our approach consists of building a database (DB) library of high-resolution IMS (HR-IMS) profiles of disaccharidic and trisaccharidic fragments. Then, the sequence of the oligosaccharide of interest is retrieved by comparing the HR-IMS profile of its disaccharidic and trisaccharide fragments with the profiles from the DB library.</p><p><strong>Results: </strong>In fact, our IMSⁿ experiments on galactomannan reveal arrival time distribution (ATD) profiles matching with known reference structures, confirming the co-existence of multiple isomers. In addition, we proved that this approach could be improved by incorporating trisaccharidic fragments to our DB library, serving in the characterization of higher degree of polymerization (DP) structures (DP4 in this case).</p><p><strong>Conclusions: </strong>Overall, this work paves the way for the characterization of even more complex oligosaccharides, which can be potentially used for bio-based material conception.</p>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":" ","pages":"e10100"},"PeriodicalIF":1.8,"publicationDate":"2025-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144625139","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Investigation of Uranyl Perchlorate Anion Complexes in the Gas Phase via Infrared Multiphoton Dissociation and Collision-Induced Dissociation","authors":"Brittany D. M. Hodges,&nbsp;JungSoo Kim,&nbsp;Giel Berden,&nbsp;Jonathan Martens,&nbsp;Christopher A. Zarzana","doi":"10.1002/rcm.10106","DOIUrl":"https://doi.org/10.1002/rcm.10106","url":null,"abstract":"<div>\u0000 \u0000 <p>The infrared multiphoton dissociation spectrum of the gas-phase uranyl perchlorate anion ([UO₂(ClO₄)₃]⁻) was measured. The asymmetric uranyl stretch lies somewhere between 930 and 1030 cm⁻¹, though it could not be deconvoluted from a closely located perchlorate stretching mode. The experimentally measured spectrum was in good agreement with spectra calculated using density functional theory with the B3LYP and TPSSh functionals and Grimme's D3 dispersion corrections with Becke–Johnson damping. The calculations suggest that the asymmetric uranyl stretch lies in the range of 970–980 cm⁻¹, about 20–30 cm⁻¹ higher than for the analogous uranyl trinitrato complex and consistent with perchlorate as a weaker ligand than nitrate. Like the uranyl trinitrato anion, fragmentation of [UO₂(ClO₄)₃]⁻ by collision-induced dissociation resulted in loss of a ClO₃^• radical to form [UO₃(ClO₄)₂]⁻. Infrared multiphoton dissociation measurements of [UO₃(ClO₄)₂]⁻ indicate that the structure of the product ion has an O⁻ ligand bound to the uranyl in a T-arrangement and two perchlorate ligands, matching the findings from uranyl nitrato complexes. The uranyl stretch in this complex was slightly separated from the perchlorate modes and was measured at 906 cm⁻¹, slightly higher than for the analogous nitrate complex, again consistent with perchlorate as a weaker ligand than nitrate in the gas phase.</p>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 20","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144615198","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Critical Method Parameters to Evaluate When Developing a Method Using a Laser Diode Thermal Desorption (LDTD) Coupled to a Mass Spectrometer","authors":"Jonathan Rochon,&nbsp;Serge Auger,&nbsp;Eshwar Jagerdeo","doi":"10.1002/rcm.10104","DOIUrl":"https://doi.org/10.1002/rcm.10104","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>This paper presents an in-depth evaluation of the laser diode thermal desorption (LDTD) device interfaced to a mass spectrometer and identifies the critical method parameters to evaluate when developing a new procedure.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Samples were solvent extracted and spotted in a 96-well plate. In the case of biological fluids, hydrolysis followed by solid phase extraction is required. The solvent in the 96-well plate is evaporated, followed by mass spectrometric analysis (MS) with atmospheric pressure chemical ionization (APCI). Where applicable, the instrument is operated in a data-dependent mode, with a full-scan mass spectrum followed by MS/MS spectra with a total runtime of 18 s per well.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Five key experiments (sample dilution, gas flow, laser ramp, ion saturation/ion suppression, and signal enhancement) were evaluated as critical parameters that could potentially be encountered in method development, and practical solutions are proposed.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Interfacing LDTD with a mass spectrometer allows for rapid screening for many analytes in a wide range of samples, with either minimal or complex sample preparation. Addressing all critical method parameters can aid in creating a sensitive and robust procedure.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 20","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144589952","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Dual-Channel Off-Axis Ion Funnel With a Deflection Electrode","authors":"Mengfei Shan,&nbsp;La Chen,&nbsp;Jun Wang,&nbsp;Luhong Wen","doi":"10.1002/rcm.10103","DOIUrl":"https://doi.org/10.1002/rcm.10103","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>In electrospray ionization mass spectrometry (ESI-MS) systems, two critical challenges persist: (1) under-expanded supersonic jets at the atmospheric pressure interface (API) cause ion losses and reduced transmission efficiency; (2) residual solvents and charged droplets entering vacuum stages lead to contamination and elevated chemical noise, degrading analysis accuracy.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>A dual-channel off-axis ion funnel with a deflection electrode (DC-OFIDE) was developed to address these challenges. This device integrates three core components: an ion drift channel (IDC), an ion funnel channel (IFC), and a deflection electrode. The IDC and IFC are separated by conjoined gaps. Ions within the gas stream emanating from the API are extracted from the IDC via a deflection field, while a retarding axial field prolongs ions' residence time, ensuring efficient transfer to the IFC. This DC-OFIDE features an enlarged entrance aperture (Φ18 mm) to accommodate a multi-capillary interface, enhancing compatibility with high-conductance sample introduction systems.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Compared with the original conventional ion funnel (CIF), the DC-OFIDE achieved a threefold enhancement in caffeine ion intensity and a broader <i>m/z</i> transmission window. It demonstrated robust neutral and droplet suppression, maintaining 80% ion intensity even under tripled serum volume infused. In drug screening of hair samples, baseline noises in drug ion peaks were reduced by 36%–82%, with a quadrupled signal-to-noise ratio improvement observed for 6-monoacetylmorphine.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>This DC-OFIDE significantly enhances ion transmission efficiency and chemical noise suppression in ESI-MS, establishing its potential for high-fidelity analysis of complex samples.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 20","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144519733","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Phytochemical Analysis of Semen Hoveniae and Its Potential Mechanism Against Alcoholic Liver Disease via an Integrated Approach Combining UHPLC-Q-TOF MS, Network Pharmacology, and Molecular Docking","authors":"Min Li,&nbsp;Zhuo-chun Wei,&nbsp;Feng-xiang Zhang,&nbsp;Hai-jun Li","doi":"10.1002/rcm.10097","DOIUrl":"https://doi.org/10.1002/rcm.10097","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Semen Hoveniae (SH), known as Zhijuzi in Chinese, is extensively utilized in China for the management of alcoholic liver disease (ALD) due to its recognized detoxification properties. Despite its extensive historical use, the detailed chemical profile and anti-ALD mechanisms of SH remain inadequately understood, significantly restricting its further therapeutic development.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>The chemical constituents of SH were systematically profiled using ultra high-performance liquid chromatography coupled with time-of-flight mass spectrometry (UHPLC-Q-TOF MS). Potential molecular targets of identified compounds were predicted using the SwissTargetPrediction platform. Common targets were subsequently analyzed via Gene Ontology (GO) and Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway enrichment analysis using the DAVID database. Network pharmacology results were validated by molecular docking.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Seventy-six compounds were identified or tentatively characterized in SH, including 50 flavonoids, 15 saponins, 5 terpenes, 3 alkaloids, 2 phenylpropanoids, and 1 other type, among which seven were unambiguously identified using reference standards. Furthermore, seven potentially novel components were identified. Network pharmacology and molecular docking analyses elucidated the molecular mechanisms underlying SH's therapeutic effects on ALD. Three core molecular targets—AKT1, SRC, and EGFR—were identified. Key pathways closely related to ALD, such as glutathione metabolism and arachidonic acid metabolism, were notably enriched, suggesting their crucial roles in SH's hepatoprotective mechanisms. Molecular docking studies confirmed strong binding affinities (binding energies lower than −5.0 kcal/mol) between six active compounds (laricetrin, apigenin, quercetin, kaempferol, myricetin, and syringetin) and the three core targets (AKT1, SRC, and EGFR).</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>This study comprehensively characterizes the chemical compositions of SH and elucidates its potential mechanisms against ALD. These findings substantiate the hepatoprotective potential of SH, providing a solid scientific foundation for its traditional use and promoting the development of novel therapeutic approaches for ALD.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 20","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144519938","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Unveiling Flavonoid Reactivity: A High-Resolution Mass Spectrometry Journey Through the Silylation of Quercetin","authors":"Thabang Bernette Ncongwane,&nbsp;Ntakadzeni Edwin Madala,&nbsp;Derek Tantoh Ndinteh,&nbsp;Elize Smit","doi":"10.1002/rcm.10101","DOIUrl":"https://doi.org/10.1002/rcm.10101","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Quercetin is an example of a pentahydroxylated flavonol compound studied extensively due to its excellent biological activity (e.g., antioxidant, antiviral, and antimicrobial). The antioxidant properties of flavonoids are influenced by the arrangement of the substituents around the molecule, a phenomenon known as the structure–activity relationship (SAR). SAR studies the relationship between compounds' structural characteristics and their biological activity in drug design.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Quercetin was silylated with MTBSTFA using a semiautomated flow system, and the order in which hydroxyl groups were silylated was used to derive the sequential reactivity of quercetin.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The collision-induced dissociation MS/MS fragmentation of the precursor ion of quercetin is influenced by the electrospray ionization (+ and − modes) and an increase in collision energy (<span>CE</span>). Structure elucidation with in-depth high-resolution tandem mass spectrometric analysis revealed that silylation primarily occurs at A7 and is sequentially followed by B3′, B4′, C3, and A5.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Retro-Dials Alder cleavage of the C-ring plays a significant role in the MS/MS fragmentations of silylated quercetin, maintaining the integrity of the fragment ions and subsequently allowing tracking of the position of the silyl group.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 20","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10101","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144519732","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}