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Investigation of the mechanism of [M–H]+ ion formation in photoionized N-alkyl-substituted thieno[3,4-c]-pyrrole-4,6-dione derivatives during higher order MSn high-resolution mass spectrometry 在高阶 MSn 高分辨率质谱分析过程中研究光离子化 N-烷基取代的噻吩并[3,4-c]吡咯-4,6-二酮衍生物中[M-H]+ 离子的形成机制。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-11-13 DOI: 10.1002/rcm.9940
Salim Sioud, Maan Amad, Zhiyong Zhu, Denis Lesage, Héloïse Dossmann
{"title":"Investigation of the mechanism of [M–H]+ ion formation in photoionized N-alkyl-substituted thieno[3,4-c]-pyrrole-4,6-dione derivatives during higher order MSn high-resolution mass spectrometry","authors":"Salim Sioud,&nbsp;Maan Amad,&nbsp;Zhiyong Zhu,&nbsp;Denis Lesage,&nbsp;Héloïse Dossmann","doi":"10.1002/rcm.9940","DOIUrl":"10.1002/rcm.9940","url":null,"abstract":"<div>\u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>The mechanism underlying dopant-assisted atmospheric pressure photoionization's (APPI) formation of ions is unclear and still under debate for many chemical classes. In this study, we reexamined the gas-phase reaction mechanisms responsible for the generation of [M–H]<sup>+</sup> precursor ions, resulting from the loss of a single hydrogen atom, in a series of <i>N</i>-alkyl-substituted thieno[3,4-<i>c</i>]-pyrrole-4,6-dione (TPD) derivatives.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Atmospheric pressure photoionization combined with higher order MS/MS<sup><i>n</i></sup> using high-resolution mass spectrometry (APPI-HR-CID-MS<sup><i>n</i></sup>) and electronic structure calculations using density functional theory were used to determine the chemical structure of observed [M–H]<sup>+</sup> ions.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>As a result, the higher order MS<sup><i>n</i></sup> (<i>n</i> = 3) experiments revealed a reversed Diels–Alder fragmentation mechanism, leading to a common fragment ion at <i>m</i>/<i>z</i> 322 from the studied [M<sub>1–5</sub>–H]<sup>+</sup> ion species. In addition, the calculation for two chemical structure models (<i>N</i>-alkyl-TPD1 and <i>N</i>-alkyl-TPD5) showed that the fragment structure, resulting from the removal of the hydrogen atom connected to the third carbon atom of the <i>N</i>-alkyl side chain, has a more stable cyclic form compared with the linear one.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The proposed chemical structure of the <i>N</i>-alkyl TPD ion species, following the loss of a single hydrogen atom, was revealed during APPI-HR-CID-MS<sup><i>n</i></sup> (<i>n</i> = 3) experiments on the [M–H]<sup>+</sup> species. Hydrogen radical (H<sup>•</sup>) abstraction from the alkyl side chain (e.g., hexyl, heptyl, octyl, 2-ethylhexyl, and nonyl) triggered a rearrangement in the radical cation structure of the <i>N</i>-alkyl-TPD derivatives, initiating cyclization and forming a six-membered ring that connects the oxygen atom to the third carbon atom in the alkyl chain. In addition, theoretical calculations supported the APPI-HR-CID-MS<sup><i>n</i></sup> (<i>n</i> = 3) experiments by demonstrating that the proposed chemical structure, resulting from the intramolecular cyclization of the <i>N</i>-alkyl-TPD ion species, was stable in the presence of chlorobenzene. These findings will aid the structural determination and elucidation of molecules with similar core structures.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 2","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-11-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142612718","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}
引用次数: 0
Development and validation of a rapid HPLC-MS/MS method for simultaneous determination of cyclosporine A and tacrolimus in whole blood for routine therapeutic drug monitoring in organ transplantation 开发并验证一种快速 HPLC-MS/MS 方法,用于同时测定全血中的环孢素 A 和他克莫司,以监测器官移植中的常规治疗药物。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-11-12 DOI: 10.1002/rcm.9932
Fei-fei Han, Hong-chuan Liu, Ting Hu, Peng-fei Li, Rui Zhao, Zhuo-ling An
{"title":"Development and validation of a rapid HPLC-MS/MS method for simultaneous determination of cyclosporine A and tacrolimus in whole blood for routine therapeutic drug monitoring in organ transplantation","authors":"Fei-fei Han,&nbsp;Hong-chuan Liu,&nbsp;Ting Hu,&nbsp;Peng-fei Li,&nbsp;Rui Zhao,&nbsp;Zhuo-ling An","doi":"10.1002/rcm.9932","DOIUrl":"10.1002/rcm.9932","url":null,"abstract":"<div>\u0000 \u0000 <section>\u0000 \u0000 <h3> Background</h3>\u0000 \u0000 <p>Therapeutic drug monitoring is an integral part of organ transplantation. A rapid, simple, economical, and robust high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneously determining the immunosuppressants cyclosporine A and tacrolimus might increase detection efficiency.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>In this study, we developed and validated a rapid HPLC-MS/MS method. Whole blood samples of 100 μL were prepared by protein precipitation with acetonitrile and 0.5 mol. L<sup>−1</sup> ZnSO<sub>4</sub>. Chromatography was performed on a pre-column using a gradient elution with 20 mmol. L<sup>−1</sup> ammonium formate and 0.1% (v/v) formic acid in water (mobile phase A) and 0.1% (v/v) formic acid in methanol (mobile phase B) at a flow rate of 1.5 mL.min<sup>−1</sup>. The analysis time was 2.2 min. Electrospray ionization and multiple reaction monitoring were performed. The lower limit of quantification was set at 1 ng. L<sup>−1</sup> for tacrolimus and 50 ng. L<sup>−1</sup> for cyclosporine A.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The method showed adequate accuracy and precision with a sufficient linear range. The calibration curve range of tacrolimus and cyclosporine A was 1–30 and 50–1500 ng·mL-<sup>1</sup>, respectively. All correlation coefficients were &gt;0.99.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The developed HPLC-MS/MS is rapid and can be used for simultaneous monitoring of tacrolimus and cyclosporine A.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 2","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-11-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142612562","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}
引用次数: 0
A fragmentation study of disaccharide flavonoid C-glycosides using triple quadrupole mass spectrometry and its application for identification of flavonoid C-glycosides in Odontosoria chinensis 利用三重四极杆质谱对双糖黄酮 C-糖苷的片段研究及其在鉴定小柴胡中黄酮 C-糖苷中的应用。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-11-09 DOI: 10.1002/rcm.9936
Bin Huang, Fangjun Chen, Xiang Zhang, Yanzhen Hu, Yuanyuan Zhang, Le Chen, Yan Meng, Ping Wen
{"title":"A fragmentation study of disaccharide flavonoid C-glycosides using triple quadrupole mass spectrometry and its application for identification of flavonoid C-glycosides in Odontosoria chinensis","authors":"Bin Huang,&nbsp;Fangjun Chen,&nbsp;Xiang Zhang,&nbsp;Yanzhen Hu,&nbsp;Yuanyuan Zhang,&nbsp;Le Chen,&nbsp;Yan Meng,&nbsp;Ping Wen","doi":"10.1002/rcm.9936","DOIUrl":"10.1002/rcm.9936","url":null,"abstract":"<div>\u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Flavonoid C-glycosides have a wide range of pharmacological activities. However, there are few mass spectrometric research on C,O-disaccharide flavonoid C-glycosides and di-C,O-saccharide flavonoid C-glycosides. Their low-energy collision-induced dissociation (ESI-CID-MS/MS) fragmentation pattern and differences have not been reported, and the fragment ion library is incomplete. Therefore, it was essential to elucidate the fragmentation patterns of disaccharide flavonoid C-glycosides, which is described in this study.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Four disaccharide flavonoid C-glycosides such as vitexin-4″-<i>O</i>-glucoside were analyzed by ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometer (UPLC-MS/MS) using electrospray ionization (ESI) in both positive and negative ion modes. Each ion and its proposed fragmentation pathways of the four disaccharide flavonoid C-glycosides were analyzed comprehensively. Finally, ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS) and the established fragmentation patterns have been used to identify disaccharide flavonoid C-glycosides in <i>Odontosoria Chinensis</i>.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The fragmentation pathways of C,O-disaccharide flavonoid C-glycosides and di-C,O-saccharide flavonoid C-glycosides are similar. They both have the mass spectrometric characteristics of O-glycoside and C-glycoside. Product ions after mixed pathways of neutral fragments such as saccharide ring fragment, O-glycosides, H<sub>2</sub>O, and CH<sub>2</sub>O elimination appeared in both types of flavonoid C-glycosides, but their relative abundances are significantly different. According to the established fragmentation patterns, di-C,O-saccharide flavonoid glycosides were also found in <i>Odontosoria chinensis</i>.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>The fragment ions at <i>m</i>/<i>z</i> 431, 413, 341, 311, 293, and 282 in negative ion mode and <i>m</i>/<i>z</i> 293, 282, 577, 559, 541, 523, 529, and 499 in positive ion mode can serves as the main characteristics for identifying C,O-disaccharide flavonoid C-glycosides and di-C,O-saccharide flavonoid C-glycosides.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 2","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142612534","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}
引用次数: 0
The environmental and health protection commitments of Jean-François Muller: Academic and societal endeavor. 让-弗朗索瓦-穆勒的环境和健康保护承诺:学术和社会努力。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-11-09 DOI: 10.1002/rcm.9938
Jean-François Gal, Pierre-Charles Maria
{"title":"The environmental and health protection commitments of Jean-François Muller: Academic and societal endeavor.","authors":"Jean-François Gal, Pierre-Charles Maria","doi":"10.1002/rcm.9938","DOIUrl":"https://doi.org/10.1002/rcm.9938","url":null,"abstract":"","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":" ","pages":"e9938"},"PeriodicalIF":1.8,"publicationDate":"2024-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142612516","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}
引用次数: 0
Two Erigeron species comparison based on their ingredient profile by UPLC-PDA-QTOF-MS/MS and discriminant analysis 通过 UPLC-PDA-QTOF-MS/MS 和判别分析,比较两种麦角菌的成分特征。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-11-04 DOI: 10.1002/rcm.9929
Jianguang Zhang, Yue Wang, Jiansang Wulu, Wenfang Jin, Qing Yang, Zhifeng Zhang
{"title":"Two Erigeron species comparison based on their ingredient profile by UPLC-PDA-QTOF-MS/MS and discriminant analysis","authors":"Jianguang Zhang,&nbsp;Yue Wang,&nbsp;Jiansang Wulu,&nbsp;Wenfang Jin,&nbsp;Qing Yang,&nbsp;Zhifeng Zhang","doi":"10.1002/rcm.9929","DOIUrl":"10.1002/rcm.9929","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p><i>Erigeron breviscapus</i> (EB) and <i>Erigeron multiradiatus</i> (EM) are the two species of the genus <i>Erigeron</i> (Asteraceae) with extremely close genetic relationships. They were used as the same “meiduoluomi” for the treatment of plague and epidemics in traditional Tibetan medicine. But in traditional Chinese medicine, only EB is used for treatment of cerebrovascular obstruction, hemiplegia due to stroke, coronary artery obstruction, chest congestion, and angina pectoris. These two <i>Erigeron</i> species show different effects in different traditional medicine systems. Therefore, analyzing the chemical compositions of two species will not only enhance comprehension of their medicinal properties but also foster the advancement and exploration of novel applications. However, to date, there has been no comprehensive and detailed investigation comparing the constituents of EB and EM.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>A methodology for rapid identification of chemical profiles from two <i>Erigeron</i> species was devised through the integration of ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-QTOF-MS/MS) and multivariate statistical analysis. Additionally, a UHPLC-photo-diode array (PDA) method was established to precisely quantify of 11 components.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>A total of 58 constituents comprising flavonoids, phenolic acids, saponin, and long chain fatty acids were elucidated. Thirteen compounds were identified as potential differentiators in chemical profiles among the two <i>Erigeron</i> species. For quantitative assessment, 11 bioactive compounds were simultaneously quantified across 49 batches of <i>Erigeron</i> species samples utilizing UHPLC-PDA with wavelengths of 325, 254, and 266 nm. The method demonstrated excellent precision, linearity, accuracy, repeatability, stability, and recovery.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The findings from this study will serve as a reference for quality control, functional activity exploration, and improved clinical application based on the ingredient profiles of the two species. Furthermore, this inaugural investigation into the ingredient profiles of these two species will enhance the potential and optimal utilization of both EB and EM resources.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 1","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142574732","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}
引用次数: 0
Optimization of protein identifications through the use of different chromatographic approaches and bioinformatic pipelines 通过使用不同的色谱方法和生物信息学管道优化蛋白质鉴定。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-11-04 DOI: 10.1002/rcm.9937
Jesus D. Castaño, Francis Beaudry
{"title":"Optimization of protein identifications through the use of different chromatographic approaches and bioinformatic pipelines","authors":"Jesus D. Castaño,&nbsp;Francis Beaudry","doi":"10.1002/rcm.9937","DOIUrl":"10.1002/rcm.9937","url":null,"abstract":"<div>\u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Selection of proteomic workflows for a given project can be a daunting task. This research provides a guide outlining the impact on protein identification of different steps such as chromatographic separation, data acquisition strategies, and bioinformatic pipelines. The data presented here will help experts and nonexpert proteomic users to increase proteome coverage and peptide identification.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>HeLa protein digests were analyzed through different C18 chromatographic columns (15 and 50 cm in length), using top 12 data-dependent acquisition (DDA), top 20 DDA, and data-independent acquisition (DIA) with a nanospray source in positive mode in a Thermo Q Exactive instrument. The raw data were analyzed using different search engines, rescoring approaches, and multi-engine searches. The results were analyzed in the context of peptide and protein identifications, precursor properties, and computation requirements to understand the differences between methods.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Our results showed that higher column lengths and top <i>N</i> DDA approaches were able to significantly increase protein identifications. The use of multiple search engines yielded limited gains, whereas the use of rescoring methods clearly outperformed other strategies. Finally, DIA approaches, although successful at generating new identifications, had a limited performance influenced by the previous collection of DDA data, which could prohibitively increase instrument time. Nonetheless, the use of library-free methods showed promising results.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Our results highlight the impact of different experimental approaches on proteome coverage. Changes in chromatographic columns, data acquisition, or bioinformatic analysis can significantly increase the number of protein identifications (&gt;400%). Thus, this research provides a reference upon which to build a successful proteomic workflow with different considerations at every step.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 1","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.9937","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142574730","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}
引用次数: 0
Triple-oxygen isotopes of stony micrometeorites by secondary ion mass spectrometry (SIMS): Olivine, basaltic glass and iron oxide matrix effects for sensitive high-mass resolution ion microprobe-stable isotope (SHRIMP-SI) 利用二次离子质谱(SIMS)分析石质微陨石的三氧同位素:橄榄石、玄武岩玻璃和氧化铁基质对灵敏度高、质量分辨率高的离子微探针-稳定同位素(SHRIMP-SI)的影响。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-10-30 DOI: 10.1002/rcm.9921
Seann J. McKibbin, Janaína N. Ávila, Trevor R. Ireland, Matthias Van Ginneken, Bastien Soens, Flore Van Maldeghem, Matthew Huber, Leonardo Baeza, Aditya Patkar, Frank Vanhaecke, Vinciane Debaille, Philippe Claeys, Steven Goderis
{"title":"Triple-oxygen isotopes of stony micrometeorites by secondary ion mass spectrometry (SIMS): Olivine, basaltic glass and iron oxide matrix effects for sensitive high-mass resolution ion microprobe-stable isotope (SHRIMP-SI)","authors":"Seann J. McKibbin,&nbsp;Janaína N. Ávila,&nbsp;Trevor R. Ireland,&nbsp;Matthias Van Ginneken,&nbsp;Bastien Soens,&nbsp;Flore Van Maldeghem,&nbsp;Matthew Huber,&nbsp;Leonardo Baeza,&nbsp;Aditya Patkar,&nbsp;Frank Vanhaecke,&nbsp;Vinciane Debaille,&nbsp;Philippe Claeys,&nbsp;Steven Goderis","doi":"10.1002/rcm.9921","DOIUrl":"10.1002/rcm.9921","url":null,"abstract":"<div>\u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Micrometeorites are extraterrestrial particles smaller than ~2 mm in diameter, most of which melted during atmospheric entry and crystallised or quenched to form ‘cosmic spherules’. Their parentage among meteorite groups can be inferred from triple-oxygen isotope compositions, for example, by secondary ion mass spectrometry (SIMS). This method uses sample efficiently, preserving spherules for other investigations. While SIMS precisions are improving steadily, application requires assumptions about instrumental mass fractionation, which is controlled by sample chemistry and mineralogy (matrix effects).</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>We have developed a generic SIMS method using sensitive high-mass resolution ion micro probe-stable isotope (SHRIMP-SI) that can be applied to finely crystalline igneous textures as in cosmic spherules. We correct for oxygen isotope matrix effects using the bulk chemistry of samples obtained by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and model bulk chemical compositions as three-component mixtures of olivine, basaltic glass and Fe-oxide (magnetite), finding a unique matrix correction for each target.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Our first results for cosmic spherules from East Antarctica compare favourably with established micrometeorite groups defined by precise and accurate but consumptive bulk oxygen isotope methods. The Fe-oxide content of each spherule is the main control on magnitude of oxygen isotope ratio bias, with effects on δ<sup>18</sup>O up to ~6‰. Our main peak in compositions closely coincides with so-called ‘Group 1’ objects identified by consumptive methods.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The magnitude of SIMS matrix effects we find is similar to the previous intraspherule variations, which are now the limiting factor in understanding their compositions. The matrix effect for each spherule should be assessed quantitatively and individually, especially addressing Fe-oxide content. We expect micrometeorite triple-oxygen isotope compositions obtained by SIMS to converge on the main clusters (Groups 1 to 4) after correction firstly for magnetite content and secondarily for other phases (e.g., basaltic glass) in each target.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 1","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.9921","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142542428","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}
引用次数: 0
Identification and characterization of alkaline hydrolytic degradation products of ivacaftor by UPLC-PDA and UPLC-ESI-QTOF-MS techniques 利用 UPLC-PDA 和 UPLC-ESI-QTOF-MS 技术鉴定和表征伊伐卡夫多的碱性水解降解产物。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-10-30 DOI: 10.1002/rcm.9930
Aastha Bishnoi, Alka Bali, Akshay Kumar
{"title":"Identification and characterization of alkaline hydrolytic degradation products of ivacaftor by UPLC-PDA and UPLC-ESI-QTOF-MS techniques","authors":"Aastha Bishnoi,&nbsp;Alka Bali,&nbsp;Akshay Kumar","doi":"10.1002/rcm.9930","DOIUrl":"10.1002/rcm.9930","url":null,"abstract":"<div>\u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>The study of inherent stability characteristics of drugs has been advocated to be important by various regulatory agencies like the ICH, USFDA, and others. The current work was envisaged to investigate the forced degradation profile of the drug ivacaftor under ICH-prescribed stress conditions, identification of its potential degradants, and postulation of the degradation routes for their generation.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>The stress degradation studies were performed on the drug as per the ICH guideline Q1A(R2). A UPLC-photodiode array-based chromatographic method was developed to satisfactorily resolve the drug from its degradation products, validated in accordance with various ICH prescribed parameters, and assessed for its BAGI practicality index. The degradation products were identified and characterized by UPLC-ESI-QTOF-MS studies.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The drug was found to significantly degrade under conditions of alkaline hydrolytic stress and it was found to be stable under all other stressor environments including acid/neutral hydrolytic, photolytic, thermal, and oxidative stress. Four alkaline hydrolytic degradation products (I-IV) were revealed by UPLC-QTOF-MS studies which were well-resolved from the drug over a C18 UPLC column by the developed UPLC-PDA method. The detection wavelength was selected as 310 nm. Characterization of the four degradation products (I–IV) was carried out by their mass spectral data and their respective degradation routes were elucidated.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>A UPLC-PDA method was developed and validated for ivacaftor and its practicality BAGI index was computed. Four alkaline hydrolytic degradation products of ivacaftor were revealed through UPLC-ESI-QTOF-MS studies and corresponding degradation routes were elucidated.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 1","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142542427","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}
引用次数: 0
How do cocaine and morphine in methanol solution desorb at the last moment of Leidenfrost phenomenon-assisted thermal desorption? 甲醇溶液中的可卡因和吗啡如何在莱顿弗罗斯特现象辅助热脱附的最后时刻脱附?
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-10-30 DOI: 10.1002/rcm.9933
Kenzo Hiraoka, Stephanie Rankin-Turner, Dilshadbek T. Usmanov, Sherzod M. Akhmedov, Satoshi Ninomiya
{"title":"How do cocaine and morphine in methanol solution desorb at the last moment of Leidenfrost phenomenon-assisted thermal desorption?","authors":"Kenzo Hiraoka,&nbsp;Stephanie Rankin-Turner,&nbsp;Dilshadbek T. Usmanov,&nbsp;Sherzod M. Akhmedov,&nbsp;Satoshi Ninomiya","doi":"10.1002/rcm.9933","DOIUrl":"10.1002/rcm.9933","url":null,"abstract":"<div>\u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>The objective of the present study is to investigate desorption of low-volatility analytes in Leidenfrost phenomenon-assisted thermal desorption (LPTD).</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>LPTD was investigated for 5 μL solutions of 0.03 ppm cocaine or morphine in methanol (sample weight: 0.12 ng) by using heated metal surfaces (240°C) polished by abrasives with grit numbers from #5000 (~3 μm) to #100 (~200 μm).</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The analyte signals were detected only after the complete evaporation of methanol solvent and the formed analyte residues levitated on the heater surface. The strongest ion signals were obtained with grit number #100.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Because the analyte residue does not come into contact with the heated surface but levitates on the hot substrate after the evaporation of the solvent, thermal decomposition of the analyte is largely suppressed. This is a great merit of LPTD for trace analysis of low-volatility and thermally labile compounds.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 1","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142542426","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}
引用次数: 0
A novel analytical strategy based on gas chromatography-Orbitrap high-resolution mass spectrometry combined with solid-phase extraction for the monitoring of stanozolol misuse in human urine 一种基于气相色谱-轨道阱高分辨质谱法并结合固相萃取的新型分析策略,用于监测人体尿液中滥用司坦唑醇的情况。
IF 1.8 3区 化学
Rapid Communications in Mass Spectrometry Pub Date : 2024-10-30 DOI: 10.1002/rcm.9935
Siying Zheng, Ziyi Ji, Yuqi Ge, Xian Fang, Mengpan Liu, Haoyi Sun, Xiaojun Deng, Lei Liao
{"title":"A novel analytical strategy based on gas chromatography-Orbitrap high-resolution mass spectrometry combined with solid-phase extraction for the monitoring of stanozolol misuse in human urine","authors":"Siying Zheng,&nbsp;Ziyi Ji,&nbsp;Yuqi Ge,&nbsp;Xian Fang,&nbsp;Mengpan Liu,&nbsp;Haoyi Sun,&nbsp;Xiaojun Deng,&nbsp;Lei Liao","doi":"10.1002/rcm.9935","DOIUrl":"10.1002/rcm.9935","url":null,"abstract":"<div>\u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Stanozolol, an anabolic androgenic steroid listed in Part S1 of the World Anti-Doping Agency Prohibited List, exhibits a low response and significant matrix interference in urine samples when using liquid–liquid extraction–gas chromatography–mass spectrometry (GC–MS). Enhancing sample preparation techniques remains essential for the effective detection of stanozolol and its metabolites.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>A method for determining stanozolol and its metabolites (3′-OH-stanozolol, 4β-OH-stanozolol, and 16β-OH-stanozolol) in human urine was developed and validated using GC-Orbitrap high-resolution MS combined with optimized mixed-mode solid-phase extraction (SPE). This method was applied to urine samples from two volunteers who orally administered a single dose of stanozolol, with samples collected over a 30-day period post-administration.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The optimized mixed-mode SPE method reduced matrix interference and achieved satisfactory extraction efficiency and high sensitivity, enabling confident identification of all targets in human urine. Validation showed extraction recovery of 74% to 81% and limits of detection from 0.1 to 0.25 ng mL<sup>−1</sup>. The method was successfully applied to detect urinary excretion profiles of stanozolol and its metabolites in positive volunteer samples.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>This study presents a novel detection protocol for stanozolol and its metabolites, enhancing the monitoring of stanozolol abuse and contributing to the integrity of sports competitions. This protocol offers a robust tool for anti-doping laboratories, aiding in the accurate detection of stanozolol misuse and supporting the enforcement of fair play in athletics.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 1","pages":""},"PeriodicalIF":1.8,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142542424","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}
引用次数: 0
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