Journal of the American Society for Mass Spectrometry最新文献

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Detection and Characterization of Cyanometabolite Complexes between Microcystin-RR and a Microguanidine by UHPLC-ESI-MS UHPLC-ESI-MS检测微囊藻毒素与微量胍之间的氰代谢复合物及表征
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-25 DOI: 10.1021/jasms.5c00165
Sanduni H. Premathilaka,  and , Dragan Isailovic*, 
{"title":"Detection and Characterization of Cyanometabolite Complexes between Microcystin-RR and a Microguanidine by UHPLC-ESI-MS","authors":"Sanduni H. Premathilaka,&nbsp; and ,&nbsp;Dragan Isailovic*,&nbsp;","doi":"10.1021/jasms.5c00165","DOIUrl":"https://doi.org/10.1021/jasms.5c00165","url":null,"abstract":"<p >Microcystins (MCs) are hepatotoxic cyclic peptides produced by cyanobacteria, with MC-RR being one of the most polar and commonly detected MC congeners in water collected during cyanobacterial harmful algal blooms (cHABs). Microguanidines (MGDs) are sulfated metabolites produced by <i>Microcystis</i> sp. that have not been reported during Lake Erie cHABs. Herein, both MGD AL772 (also abbreviated here as MGD) and previously unreported complex ions containing MC-RR and MGD AL772 were discovered after UHPLC-ESI-HRMS, MS/MS, and MS/MS/MS analyses of the Lake Erie cHAB samples in positive and negative modes. Initially, a triply charged [(MC-RR)<sub>2</sub>-MGD+3H]<sup>3+</sup> ion was detected at the same retention time as coeluting [MC-RR+2H]<sup>2+</sup> and [MGD-H]<sup>−</sup> ions. Characterization of this complex ion by HCD, CID, ETD and thiol derivatization indicates that two [MC-RR+2H]<sup>2+</sup> ions are bonded to one [MGD-H]<sup>−</sup>, probably through interactions of positively charged guanidinium groups of arginine (R) residues and negatively charged MGD’s sulfate groups, to form the triply charged complex during ESI. Four other complexes, including [MC-RR-MGD] and its in-source fragment [(MC-RR-MGD)-SO<sub>3</sub>], were also detected as positive and negative ions at the same time due to coelution of MC-RR and MGD. These findings not only underscore the importance of an efficient separation for quantification of cyanobacterial metabolites but also provide novel insights into their interactions during ESI, which enabled the present report on the complexes between MC-RR and a sulfated cyanobacterial metabolite, MGD AL772.</p>","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 9","pages":"1950–1958"},"PeriodicalIF":2.7,"publicationDate":"2025-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144929034","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
Active Humidity Control Chamber for Desorption Electrospray Ionization-Mass Spectrometry Imaging Applications 主动湿度控制室解吸电喷雾电离质谱成像应用
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-22 DOI: 10.1021/jasms.5c00111
Hawkins S. Shepard, Robert L. G. Gottschalk, Jody C. May and John A. McLean*, 
{"title":"Active Humidity Control Chamber for Desorption Electrospray Ionization-Mass Spectrometry Imaging Applications","authors":"Hawkins S. Shepard,&nbsp;Robert L. G. Gottschalk,&nbsp;Jody C. May and John A. McLean*,&nbsp;","doi":"10.1021/jasms.5c00111","DOIUrl":"https://doi.org/10.1021/jasms.5c00111","url":null,"abstract":"<p >Ambient ionization techniques enable mass spectrometry (MS) to expand into broader experimental contexts, although it is increasingly clear that results are influenced by the environmental conditions at the site of sampling. Desorption electrospray ionization (DESI), in particular, is affected by variations in relative humidity (RH) levels. Here we describe the design, development, and construction of an environmental control chassis that can actively modulate RH within ± 3% of user-defined set points across a broad humidity range (15%–70% RH). Preliminary characterization demonstrated differential analyte responses across a range of set points, with observed enhancement of leucine-enkephalin, sulfadimethoxine (negative mode), and maltose (positive mode) in response to increased humidity. The measurable differences in analyte signals across discrete humidity set points underscore the importance of environmental control in ambient ionization strategies. The humidity control system outlined here can be translated to other DESI platforms, with construction information provided herein.</p>","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 9","pages":"1995–1999"},"PeriodicalIF":2.7,"publicationDate":"2025-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.acs.org/doi/pdf/10.1021/jasms.5c00111","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144929054","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Combined Trapped Ion Mobility and Infrared Ion Spectroscopy Study of Protonation Sites in Aromatic Amines 芳香胺中质子化位点的捕获离子迁移率和红外离子光谱联合研究
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-21 DOI: 10.1021/jasms.5c00164
Laura Finazzi, Lara van Tetering, Jelle L. Schuurman, Jonathan Martens, Giel Berden and Jos Oomens*, 
{"title":"Combined Trapped Ion Mobility and Infrared Ion Spectroscopy Study of Protonation Sites in Aromatic Amines","authors":"Laura Finazzi,&nbsp;Lara van Tetering,&nbsp;Jelle L. Schuurman,&nbsp;Jonathan Martens,&nbsp;Giel Berden and Jos Oomens*,&nbsp;","doi":"10.1021/jasms.5c00164","DOIUrl":"https://doi.org/10.1021/jasms.5c00164","url":null,"abstract":"<p >The protonation site of aromatic amines in the gas phase has been under substantial debate, as it involves a subtle competition between the higher electronegativity of the amine nitrogen and the better charge delocalization ability of the fused aromatic rings. Previous studies have unambiguously shown, especially by ion mobility measurements, that higher-energy tautomers are easily observed depending on the experimental conditions in the ion source, including voltage settings and the type of solvent used in spray sources. Here, we use a combination of ion mobility and ion spectroscopy and focus on the tautomeric structure <i>after</i> ion mobility separation, in particular for protonated 1-aminonaphthalene and 1-aminoanthracene. We employ an atmospheric pressure chemical ionization (APCI) source, with a direct insertion probe to avoid any solvent influence, mounted on an FTICR mass spectrometer with a trapped ion mobility (TIMS) unit and optical access to the ions to perform infrared (IR) multiple-photon dissociation spectroscopy using the Free-Electron Laser for Infrared eXperiments (FELIX). TIMS analysis indeed reveals the presence of both N- and C-protonated species, but the IR spectra recorded in the ICR cell also suggest that mobilization and scrambling of the proton occur after TIMS separation. We computationally investigate the energetics of tautomerization and experimentally explore ion activation after TIMS separation.</p>","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 9","pages":"1940–1949"},"PeriodicalIF":2.7,"publicationDate":"2025-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.acs.org/doi/pdf/10.1021/jasms.5c00164","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144929063","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Faces of Mass Spectrometry/Pratik Jagtap. 质谱的面孔/Pratik Jagtap。
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-21 DOI: 10.1021/jasms.5c00264
Anne Brenner, J D Brookbank
{"title":"Faces of Mass Spectrometry/Pratik Jagtap.","authors":"Anne Brenner, J D Brookbank","doi":"10.1021/jasms.5c00264","DOIUrl":"https://doi.org/10.1021/jasms.5c00264","url":null,"abstract":"","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":" ","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144938356","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
Collision-Induced Unfolding of High-m/z Native-like Protein Ions within a Trapped Ion Mobility Spectrometer 高m/z原生蛋白离子在捕获离子迁移谱仪中的碰撞诱导展开
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-21 DOI: 10.1021/jasms.5c00246
Olakunle O. Akinola,  and , Nicholas B. Borotto*, 
{"title":"Collision-Induced Unfolding of High-m/z Native-like Protein Ions within a Trapped Ion Mobility Spectrometer","authors":"Olakunle O. Akinola,&nbsp; and ,&nbsp;Nicholas B. Borotto*,&nbsp;","doi":"10.1021/jasms.5c00246","DOIUrl":"https://doi.org/10.1021/jasms.5c00246","url":null,"abstract":"<p >Native mass spectrometry (nMS) is a powerful tool for the rapid characterization of protein ions and protein–ligand complexes. By coupling nMS with ion mobility spectrometry (IMS), and collisional activation, we can rapidly obtain insights into protein conformation, and stability can be rapidly obtained. Originally incapable of this workflow, recent work enabled this collision-induced unfolding (CIU) process on commercially available Bruker timsTOF instruments. This early work, however, faced challenges in transmitting larger proteins and sought to unfold only small proteins up to 29 kDa. In this study, we continue the development of this technique and optimized instrument settings to enable the transmission of proteins up to 8,000 Th. The technique also demonstrates the capability to sufficiently energize ions to unfold native-like dimers of superoxide dismutase and β-lactoglobulin and the 45 kDa monomeric ovalbumin. When this TIMS activation technique is applied to large protein ions, however, limited unfolding was observed for bovine serum albumin, and no unfolding was observed for immunoglobulin G likely reflecting the limit of activation for this workflow.</p>","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 9","pages":"1988–1994"},"PeriodicalIF":2.7,"publicationDate":"2025-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144929138","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
Multipass CCS Refiner: A Web Application for Accurate Collision Cross Section Calibration in Cyclic Ion Mobility-Mass Spectrometry 多通道CCS精炼厂:循环离子迁移-质谱法中精确碰撞截面校准的Web应用程序。
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-19 DOI: 10.1021/jasms.5c00199
Eric C. Gier, Dmitry Leontyev and Facundo M. Fernández*, 
{"title":"Multipass CCS Refiner: A Web Application for Accurate Collision Cross Section Calibration in Cyclic Ion Mobility-Mass Spectrometry","authors":"Eric C. Gier,&nbsp;Dmitry Leontyev and Facundo M. Fernández*,&nbsp;","doi":"10.1021/jasms.5c00199","DOIUrl":"10.1021/jasms.5c00199","url":null,"abstract":"<p >In this paper, we present the <i>Multipass CCS Refiner</i>, an R application for calibrating multipass collision cross section (CCS) measurements with cyclic ion mobility spectrometry (cIMS). The <i>Multipass CCS Refiner</i> combines the necessary tools for calculating accurate CCS measurements from multipass cIMS experiments into a user-friendly web-based Shiny interface accessible regardless of programming knowledge. The application provides a suite of functions for calculating accurate arrival times, automated pass counting approximation, correction of arrival time perturbations during separation, constructing calibration curves unique to specific instrument settings, separating fine mobility features, and a variety of visualization tools. Code for the application is structured to be easily modified to meet the user’s needs. The <i>Multipass CCS Refiner</i> implements the calibration approach described by Lin and Costello to reduce the need for carefully selected separation times while accounting for artifacts underlying fluctuations in measured ion arrival times. The application is showcased with downloadable data files of commonly used standards, which can be run in the app directly or edited with user experimental data.</p>","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 9","pages":"2000–2004"},"PeriodicalIF":2.7,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.acs.org/doi/pdf/10.1021/jasms.5c00199","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144881774","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Faces of Mass Spectrometry/Kylie Bemis 质谱分析的面孔/Kylie Bemis。
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-18 DOI: 10.1021/jasms.5c00225
Anne Brenner, J.D. Brookbank and Kylie Bemis, 
{"title":"Faces of Mass Spectrometry/Kylie Bemis","authors":"Anne Brenner,&nbsp;J.D. Brookbank and Kylie Bemis,&nbsp;","doi":"10.1021/jasms.5c00225","DOIUrl":"10.1021/jasms.5c00225","url":null,"abstract":"","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 9","pages":"1845–1848"},"PeriodicalIF":2.7,"publicationDate":"2025-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144870788","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
The Protective Effects of CO2 on Fragile Ions in Differential Mobility Spectrometry 差分迁移率光谱法研究CO2对脆弱离子的保护作用。
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-18 DOI: 10.1021/jasms.5c00098
Andrew L. Finlay, Wojciech Gabryelski and W. Scott Hopkins*, 
{"title":"The Protective Effects of CO2 on Fragile Ions in Differential Mobility Spectrometry","authors":"Andrew L. Finlay,&nbsp;Wojciech Gabryelski and W. Scott Hopkins*,&nbsp;","doi":"10.1021/jasms.5c00098","DOIUrl":"10.1021/jasms.5c00098","url":null,"abstract":"<p >We explore the protective effects of adding CO<sub>2</sub> to the N<sub>2</sub> carrier gas when we conduct differential mobility spectrometry (DMS) analysis of fragile ions. A selection of fragile analytes of varying chemistries were chosen from our lab inventory and include protonated glycine, methylbenzyl ammonium, methoxybenzylpyridinium, the protonated 2-pentanone dimer, deprotonated GenX (a perfluoroalkyl substance; PFAS), and deprotonated trifluoroacetic acid. By raising the separation voltage or the carrier gas temperature, conditions were set to induce fragmentation of the analyte ions within the DMS collision cell. Subsequently introducing CO<sub>2</sub> into the N<sub>2</sub> carrier gas at concentrations ranging from 10 – 70% mitigated ion fragmentation and resulted in signal intensity gains of multiple orders of magnitude. Interestingly, stabilization of the fragile ions sometimes occurred without introducing significant ionogram peak shifts (i.e., shifts of less than 1 V), indicating that these ions exhibit relatively weak interactions with the CO<sub>2</sub> modifier. Electronic structure calculations yield Gibbs binding energies of <i>ca</i>. – 1 kJ mol<sup>–1</sup> under the DMS conditions employed, further supporting the hypothesis that dynamic ion-CO<sub>2</sub> clustering is not the root cause of the observed protective effect. The addition of CO<sub>2</sub> was also found to stabilize noncovalently bound dimers, presumably generated at the ionization source. These results indicate that, in these examples, CO<sub>2</sub> cools the ions in the energetic DMS environment via momentum transfer and energy partitioning, and that introducing CO<sub>2</sub> into DMS gas mixtures could enable the stabilization, separation, and analysis of fragile analytes.</p>","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 9","pages":"1860–1868"},"PeriodicalIF":2.7,"publicationDate":"2025-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144870789","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
Dissecting Interactions between RNA and Coronavirus Nucleocapsid Proteins Using Native Mass Spectrometry 利用天然质谱分析RNA与冠状病毒核衣壳蛋白之间的相互作用。
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-17 DOI: 10.1021/jasms.5c00159
Virginia K. James, Olivia E. Dioli and Jennifer S. Brodbelt*, 
{"title":"Dissecting Interactions between RNA and Coronavirus Nucleocapsid Proteins Using Native Mass Spectrometry","authors":"Virginia K. James,&nbsp;Olivia E. Dioli and Jennifer S. Brodbelt*,&nbsp;","doi":"10.1021/jasms.5c00159","DOIUrl":"10.1021/jasms.5c00159","url":null,"abstract":"<p >The nucleocapsid protein is the most abundant protein in the SARS-CoV virus and plays critical roles in RNA packaging and storage, yet the nature of the protein’s interactions with RNA remain elusive owing to the presence of multiple disordered regions of the protein. Here we evaluate the protein–RNA and protein–protein interactions of nucleocapsid proteins from the SARS-CoV-1 WT, SARS-CoV-2 WT, and SARS-CoV-1 omicron to better understand how the interactions are modulated by sequence variations. By using native mass spectrometry, we reveal that all three nucleocapsid proteins exist as both monomers and dimers that bind up to two RNA molecules per monomer, suggesting dual RNA binding sites. Ultraviolet photodissociation (UVPD) was used to localize the RNA binding sites found in the RNA binding domain and N-terminus of the nucleocapsid protein. The stabilities of the dimer complexes of the three nucleocapsid were monitored using energy-variable collision-induced dissociation, revealing that the dimer from SARS-CoV-1 is less stable than the dimers of the other two SARS-CoV variants in the gas phase. Furthermore, variable temperature electrospray ionization (ESI) experiments of the RNA-bound nucleocapsid proteins indicated that the protein–RNA interactions are stronger than the protein–protein interactions in solution as the dimeric protein–RNA complexes dissociate into monomeric protein–RNA complexes prior to the loss of RNA.</p>","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 9","pages":"1921–1928"},"PeriodicalIF":2.7,"publicationDate":"2025-08-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144870787","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
Faces of Mass Spectrometry/Tabiwang Arrey 质谱分析的面孔/Tabiwang Arrey。
IF 2.7 2区 化学
Journal of the American Society for Mass Spectrometry Pub Date : 2025-08-15 DOI: 10.1021/jasms.5c00262
Anne Brenner,  and , J. D. Brookbank, 
{"title":"Faces of Mass Spectrometry/Tabiwang Arrey","authors":"Anne Brenner,&nbsp; and ,&nbsp;J. D. Brookbank,&nbsp;","doi":"10.1021/jasms.5c00262","DOIUrl":"10.1021/jasms.5c00262","url":null,"abstract":"","PeriodicalId":672,"journal":{"name":"Journal of the American Society for Mass Spectrometry","volume":"36 10","pages":"2013–2016"},"PeriodicalIF":2.7,"publicationDate":"2025-08-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144854159","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
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