Rapid Communications in Mass Spectrometry最新文献

{"title":"Exploring the Mechanisms of Cyclosporine Therapy in Aplastic Anemia: A Data-Independent Acquisition Proteomics Approach","authors":"Mingxin Guo,&nbsp;Ting Dai,&nbsp;Lin Wan,&nbsp;Xiang Sun,&nbsp;Zhiqiang Hu,&nbsp;Yanchun Chen","doi":"10.1002/rcm.10085","DOIUrl":"https://doi.org/10.1002/rcm.10085","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Clinically, cyclosporine (CsA) plays a crucial role in the treatment of aplastic anemia (AA) and has demonstrated significant therapeutic efficacy. We applied DIA-based quantitative proteomics to analyze plasma protein profiles in AA patients, aiming to identify proteins and pathways modulated by CsA, thereby elucidating its therapeutic mechanisms.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Plasma samples from three AA patients pre– and post–CsA treatment underwent data-independent acquisition proteomics. DEPs were identified using fold-change thresholds. Gene Ontology, KEGG, and STRING analyses revealed functional pathways and hub proteins, which were validated by ELISA in 13 AA patients. Molecular docking assessed CsA-core protein binding affinities.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Compared to healthy people, AA patients exhibited 303 differential proteins, enriched in pathways related to oxidative stress, cellular adhesion, and energy dysregulation. Post–CsA treatment, 107 DEPs were identified, linked to redox balance and structural remodeling. Forty-eight proteins overlapped, with GAPDH, SOD1, CFL1, and ACTG1 as core targets. ELISA confirmed expression differences, and molecular docking showed strong CsA binding affinities to these proteins.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Significant protein expression differences between AA patients and healthy controls suggest immune-related pathways, including metabolism, oxidative stress, and cell structure, as key treatment targets. CsA may regulate these to intervene in AA progression.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 17","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144171539","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":"Structural Elucidation of a Unique Glycerophospho Lipid A From Phenol-Phase Soluble Lipopolysaccharide of Vibrio anguillarum Serovar SJ-41","authors":"Trevena N. Youssef,&nbsp;Abanoub Mikhael,&nbsp;David R. Goodlett,&nbsp;Travis D. Fridgen,&nbsp;Joseph Banoub","doi":"10.1002/rcm.10083","DOIUrl":"https://doi.org/10.1002/rcm.10083","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>In this study, the chemical structure of a unique lipid A derived from the phenol-phase soluble lipopolysaccharide (LPS) of <i>Vibrio anguillarum</i> serovar SJ-41, a virulent marine and freshwater pathogen, was investigated using electrospray ionization with field asymmetric wave ion mobility-Orbitrap mass spectrometry (ESI-FAIMS-MS). The analysis indicated that the obtained lipid A consisted of a heterogeneous mixture of molecules. High-energy collision dissociation tandem mass spectrometry (HCD-MS/MS) allowed the identification of unique chemical motifs of <i>V. anguillarum</i> lipid A.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>ESI-FAIMS-MS, HCD-MS/MS, and Kendrick mass defect (KMD) plots were used to elucidate <i>V. anguillarum</i> lipid A molecular structure and mixture heterogeneity.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Structural analysis revealed significant deviations from canonical lipid A, including the presence of a phospho-glycerol moiety located on primary acyl chain at the O-3 position of reducing sugar end and presence of novel di-hydroxylated primary acyl chains on the N-2′ position of the non-reducing sugar end. As far as we know, this is the first report of lipid A structures containing both phospho-glycerol moiety and di-hydroxylated primary acyl chains. KMD plots were employed to investigate structural diversity of lipid A complex mixture.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Tandem mass spectrometric analyses and KMD plots allowed the determination of lipid A structural diversity. These findings provide new insights into the lipid A composition of <i>V. anguillarum</i> strain SJ-41 and underscore the need for further studies to explore its biological implications, potentially reshaping our understanding of lipid A and its role in host-pathogen interactions.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 17","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144171966","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":"Exploration of Different Pre-Processing and Drying Methods on Volatile Organic Compounds in Bletilla striata Based on GC-IMS","authors":"Rui Xu,&nbsp;Shanshan Wang,&nbsp;Yiyuan Luo,&nbsp;Ping Pan,&nbsp;Yitian Zhao,&nbsp;Juan Wang,&nbsp;Hongjiang Chen","doi":"10.1002/rcm.10082","DOIUrl":"https://doi.org/10.1002/rcm.10082","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p><i>Bletilla striata</i> (Thunb.) Rchb.f. (Orchidaceae), a traditional Chinese medicine herb known as baiji, exhibits diverse pharmacological activities. Despite extensive research on its phytochemistry, the volatile organic compounds (VOCs) of <i>B. striata</i> remain largely unexplored.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Gas chromatography-ion mobility spectrometry (GC-IMS) was used to analyze and compare the VOCs of three pre-processing methods (fresh, boiling, and steaming) and four drying methods (sun-drying [SD], vacuum freeze drying [VFD], hot air drying [HAD], microwave drying [MD]) in <i>B. striata</i>.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>A total of 137 VOCs were detected and 124 VOCs were identified, primarily including aldehydes, alcohols, and ketones. Principal component analysis (PCA) and fingerprint similarity analysis revealed that the drying method has a greater impact on VOCs than pre-processing method. Partial least squares-discriminant analysis (PLS-DA) and heat map cluster analysis identified 34 VOCs as main characteristic markers to differentiate the samples of <i>B. striata</i> with different processing methods. Additionally, the samples subjected to sequential steaming followed by sun-drying demonstrated a superior ability to retain both the quantity and variety of non-harmful VOC.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>This research conducted a detailed analysis of the fundamental VOCs in <i>B. striata</i> and provided a scientific theoretical guidance for optimizing processing of <i>B. striata</i> medicinal materials.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 17","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144171540","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":"Study of the Photoinduced Fate of Selected Contaminants in Surface Waters by HPLC-HRMS","authors":"Rossella Sesia,&nbsp;Federica Dal Bello,&nbsp;Claudio Medana,&nbsp;Rita Binetti,&nbsp;Dimitra Papagiannaki,&nbsp;Paola Calza","doi":"10.1002/rcm.10075","DOIUrl":"https://doi.org/10.1002/rcm.10075","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Photoinduced transformation of contaminants of emerging concern (CECs) can occur in aquatic environment and could lead to the formation of transformation products (TPs) of greater concern than the parent compounds. For such, the fate of epoxiconazole, hymecromone, and coumarin in water was investigated by simulating photoinduced abiotic transformations to assess the toxicity of their TPs and which CEC may be of greatest concern.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Heterogeneous photocatalysis with TiO₂ and direct photolysis of selected CECs were exploited to simulate their TPs. The TPs were assessed by means of HPLC coupled with an Orbitrap MS analyser in ESI positive mode, while their toxicity was evaluated through a <i>Vibrio fischeri</i> bioluminescence assay, and ECOSAR tool.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The formation of numerous TPs via different photoinduced pathways was noticed (27 for epoxiconazole, 6 for coumarin, and 8 for hymecromone, some of which are in the form of structural isomers). Toxicity assessment via <i>V. fischeri</i> assay showed that, unlike coumarin species, epoxiconazole transformation proceeds through the formation of toxic compounds. By means of ECOSAR software, the formation of predominant more noxious TPs of epoxiconazole was proved than the parent compound for both acute and chronic toxicities. Instead, most TPs of coumarin and hymecromone generally exhibited “harmful” and “toxic” levels of acute and chronic toxicities.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>A probable structural identification was assigned to the monitored TPs via HPLC-HRMS to recognize the several transformation pathways, of which the hydroxylation reaction was predominant, and which compound may be more hazardous in the aquatic system due to its TPs. Epoxiconazole transformation brought to potentially toxic TPs, whereas photoinduced degradation of coumarin and hymecromone resulted in less hazardous TPs. The most significant aspect of this work is the ability of this overall approach to identify the formation of photoinduced TPs that are potentially more toxic than the original CEC.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 17","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10075","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144100889","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":"Oxygen Isotope Analysis for Silicate Minerals Using a High-Temperature Conversion/Elemental Analyzer-Isotope Ratio Mass Spectrometer","authors":"Ryosuke Kikuchi,&nbsp;Tobimaru Ishiwata,&nbsp;Ichiro Tayasu","doi":"10.1002/rcm.10072","DOIUrl":"https://doi.org/10.1002/rcm.10072","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Oxygen isotope composition of silicates is an important indicator of the formation environment and/or subsequent geochemical processes of minerals. Compared to carbonate minerals and organic matter, silicate is a less common target for oxygen isotope measurements because of the need for specialized fluorination instruments to break strong Si–O bonds.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>We introduce a simple method using a high-temperature conversion elemental analyzer-isotope ratio mass spectrometer (TC/EA-IRMS), which does not require specialized instrumentation. Silicate powder with various fluorine compounds and ratios of fluorine/oxygen were decomposed at 1450°C, and then, mass spectral characteristics, oxygen yields, and δ¹⁸O values were compared.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>NaF and KF were the most reactive fluorine sources, followed by polytetrafluoroethylene, LiF, CaF₂, BaF₂, and AlF_3, with decreasing reactivity. The F/O ratio affected the tailing of the CO peaks in the mass spectrum. Higher F/O ratios show a more rapid regression to background, resulting in higher reproducibility of oxygen yield and δ¹⁸O. In addition to simply adding fluorides to the sample, homogenization treatment also improved the reactivity. Activated carbon catalyzed by nickel is a better carbon source than graphite in terms of reactivity. The quartz and smectite with NaF added at an F/O ratio of 6 provided 90.0%–99.3% of oxygen yields, δ¹⁸O values that deviated less than 1.42‰ from literature values, and 0.18‰–0.30‰ of precision.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Although further investigation is required to verify its accuracy, the potential of the TC/EA-IRMS method for silicates is demonstrated. Because the hydrogen isotope composition can also be examined using the same instrument, it is expected that this method can be applied to a wider range of earth materials, including hydrous silicates such as clay minerals.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 17","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144100888","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":"Correction to “Performance of Cryogenic Adsorbents for Use in Methane Bulk and Clumped Isotope Analysis”","authors":"","doi":"10.1002/rcm.10074","DOIUrl":"https://doi.org/10.1002/rcm.10074","url":null,"abstract":"<p>\u0000 <span>N. Kueter</span>, <span>N. Zhang</span>, <span>J. G. C. Meissner</span>, <span>L. Monnereau</span>, <span>P. M. Magyar</span>, <span>L. Emmenegger</span>, <span>S. M. Bernasconi</span>, and <span>J. Mohn</span>, “ <span>Performance of Cryogenic Adsorbents for Use in Methane Bulk and Clumped Isotope Analysis</span>,” <i>Rapid Communications in Mass Spectrometry</i>, <span>2025</span>; <span>39</span>:e10040, https://doi.org/10.1002/rcm.10040.\u0000 </p><p>The funding statement in the Acknowledgments section for this article is incorrect. The correct funding statement is shown below:</p><p>This study is supported by the Swiss National Science Foundation project no. 200021-200977 (CLUMPME) and 206021_183294 (QCL4CLUMPS). This work is part of the project 21GRD04 isoMET, which has received funding from the European Partnership on Metrology, co-financed from the European Union's Horizon Europe Research and Innovation Programme and by the Participating States. The Empa contribution has received funding from the Swiss State Secretariat for Education, Research and Innovation (SERI).</p><p>We apologize for this error.</p>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 17","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10074","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144091657","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":"A Progressive Peak-Finding and Weak Peak-Preserving LM Algorithm for Isotope Separation in Miniature Mass Spectrometers","authors":"Zhiwei Wang,&nbsp;Ang Li,&nbsp;Wei Xu,&nbsp;Dayu Li","doi":"10.1002/rcm.10073","DOIUrl":"https://doi.org/10.1002/rcm.10073","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>In recent years, performance enhancement strategies for miniature mass spectrometers through signal processing techniques have garnered significant attention, primarily due to their advantage of not changing their mechanical structure. Gaussian decomposition, as a signal processing approach, has shown considerable potential in the field of overlapping peak identification.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Method</h3>\u0000 \u0000 <p>In this study, a novel PPWP-LM (progressive peak-finding and weak peak-preserving Levenberg-Marquardt) algorithm integrating Gaussian decomposition techniques is proposed for use in miniature ion trap mass spectrometers for aliased peak separation.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Result</h3>\u0000 \u0000 <p>The feasibility of the algorithm was verified using simulation data, and the anti-noise performance of the PPWP-LM algorithm was verified under different signal-to-noise ratios. The analytical capability of the algorithm was further evaluated using samples at different concentrations and different scanning speeds, and the results showed that the algorithm maintained stable performance and was adaptable under high-speed scanning conditions. In addition, aliased signal separation was successfully demonstrated by mixing samples, and the results show that it is suitable for rapid analysis in the field and meets the requirements of practical applications.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>Through optimized strategies including a progressive search, pseudo-peak removal, and weak peak protection, the algorithm successfully achieves isotope separation under high-speed scanning conditions in miniature ion trap mass spectrometers, significantly enhancing their analytical efficiency and performance.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 17","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144091658","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":"An Improved Chemical Extraction Procedure for the Sr Isotope Analysis of Liquid Agrifood Samples Applied to Authenticating the Origin of Maple Syrups in Quebec (Canada)","authors":"B. Saar de Almeida,&nbsp;R. Stevenson,&nbsp;M. Sadiki,&nbsp;L. Lagacé,&nbsp;D. Widory","doi":"10.1002/rcm.10066","DOIUrl":"https://doi.org/10.1002/rcm.10066","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>We describe a new simplified sample preparation technique, based on dual chromatography for the analysis of ⁸⁷Sr/⁸⁶Sr in liquid agri-food samples. We applied this approach for authenticating the origin of maple syrup products in Quebec, characterizing the ⁸⁷Sr/⁸⁶Sr of soil profiles from geologically distinct maple groves, including maple tree components and maple syrup products.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>In our simplified technique, 3 mL of the organic liquids was poured into a 15-mL centrifuge tube, diluted with 10 mL of Mill-Q H₂O, and manually shaken to produce a thin juice. The thin juice was subsequently loaded in two 7.5 mL aliquots onto 10-mL Bio-RadTM chromatography columns containing 4 mL of cleaned AG50-X8 resin (100–200 mesh in a 1-N HCl solution). Once the sample was absorbed by the resin, the organic fraction of the thin juice was eluted by adding 3 × 5 mL of 1-N HCl. The Sr and other cations were subsequently recovered by adding 2 × 5 mL of 6-N HCl.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The maple groves and the ⁸⁷Sr/⁸⁶Sr ratios for maple syrup from 39 different producing areas in Quebec indicated that no isotope fractionation occurs between the syrup, the maple trees, and the corresponding labile fraction of the soil they grew upon. This suggests that ⁸⁷Sr/⁸⁶Sr provides a reliable isotope fingerprint for the provenance of maple syrups. Gathering available agri-food ⁸⁷Sr/⁸⁶Sr data across the Quebec province, we constructed the first bioavailable ⁸⁷Sr/⁸⁶Sr map based on actual agri-food data.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>This study reported an improved method for Sr separation for ⁸⁷Sr/⁸⁶Sr studies in liquids by combining two different cation-exchange chromatography steps. Data were used to develop a bioavailable ⁸⁷Sr/⁸⁶Sr map that can be used to predict the geographical origin of agrifood products from southern Quebec.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 16","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10066","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143944681","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":"LC-IRMS Persulfate Oxidation: Case Study on Neonicotinoid-Related Structures","authors":"Felix Niemann,&nbsp;Annika Gruhlke,&nbsp;Maik A. Jochmann,&nbsp;Torsten C. Schmidt","doi":"10.1002/rcm.10067","DOIUrl":"https://doi.org/10.1002/rcm.10067","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Liquid chromatography-isotope ratio mass spectrometry (LC-IRMS) is used to analyze stable carbon isotope ratios of polar nonvolatile compounds. However, challenges with the persulfate-based oxidation interface have been reported, particularly for molecules with recalcitrant structures like those found in neonicotinoids. This study systematically investigates the oxidation efficiency of neonicotinoid-related structures in a commercial LC-IRMS.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Neonicotinoid proxies of varying molecular complexity were evaluated for carbon recovery and stable carbon isotope ratio accuracy. LC-IRMS parameters such as oxidant concentration, reaction time, temperature, acid concentration, and the presence of AgNO₃ catalyst were varied. Carbon recoveries and <i>δ</i>¹³C biases were determined by injecting an oxidation-independent inorganic carbon standard under identical conditions. Elemental analyzer isotope ratio mass spectrometry (EA-IRMS) was used to normalize <i>δ</i>¹³C values.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Several neonicotinoid derivatives exhibited low carbon recovery and significant <i>δ</i>¹³C bias. Increasing oxidant concentration, reactor temperature, and reaction time improved recoveries but did not fully mitigate isotopic biases. The addition of AgNO₃ improved carbon recoveries for most derivatives but introduced variability in <i>δ</i>¹³C values, likely due to shifts in reaction mechanisms. A workflow to identify oxidation problems during method development was proposed.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Optimization of LC-IRMS oxidation parameters is critical for urea, guanidine, and nitroguanidine derivatives and similar compounds. A systematic evaluation of oxidation efficiencies under different conditions is needed for optimal mineralization and thus more accurate <i>δ</i>¹³C ratios.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 16","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10067","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143938831","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":"Dried Blood Spot Analysis for Simultaneous Quantification of Antiepileptic Drugs Using Liquid Chromatography–Tandem Mass Spectrometry","authors":"Mariam M. Abady,&nbsp;Ji-Seon Jeong,&nbsp;Ha-Jeong Kwon","doi":"10.1002/rcm.10064","DOIUrl":"https://doi.org/10.1002/rcm.10064","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Dried blood spot (DBS) sampling for the therapeutic drug monitoring of antiepileptic drugs offers practical advantages, including minimal invasiveness and ease of collection. However, for precise therapeutic management, its accuracy and reliability in quantification need to be validated.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>This study validates DBS sampling for the analysis of 11 antiepileptic drugs using liquid chromatography-tandem mass spectrometry (LC-MS/MS), overcoming the physicochemical challenges associated with DBS samples.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The acetonitrile-based DBS extraction method demonstrated high efficiency for the 11 antiepileptic drugs. Accuracy and precision within 6% were achieved in both intra- and inter-day assays, with good selectivity, minimal matrix effects, and negligible carryover. All antiepileptic drugs exhibited stability in DBS samples for at least 30 days at room temperature, confirming proper handling and storage of the DBS samples. A 3 mm diameter disc punched from a DBS produced accurate results for all target drugs.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The optimized method provided a time- and cost-effective solution, showing a strong correlation between drug concentrations in whole blood, thereby supporting the suitability of DBS sampling as a promising and advanced method for antiepileptic drug monitoring.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 16","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-05-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143938830","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}