The rising incidence of Salmonella-induced diarrhea highlights the critical need for judicious antibiotic use to ensure effective treatment outcomes.
Methods
This study presents an innovative methodology for evaluating the susceptibility of Salmonella to ceftriaxone and azithromycin through the application of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.
Results
The proposed method requires only 2–3 individual Salmonella colonies and yields results within approximately 1 hour, assessing susceptibility to ceftriaxone (70 mg/L) and azithromycin (25 mg/L). In comparison to the Kirby-Bauer method, this technique exhibits a sensitivity of 98.64% and a specificity of 84.38%.
Conclusions
The method developed in this study is both straightforward and user-friendly, making it suitable for deployment in major laboratories equipped with time-of-flight mass spectrometry. It offers a preliminary assessment of Salmonella susceptibility to ceftriaxone and azithromycin, thereby enhancing the accuracy of clinical interventions for Salmonella infections.
{"title":"Sensitive Detection of Salmonella Susceptibility to Ceftriaxone and Azithromycin Using Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry","authors":"Guohao Zhan, Shujin Xie, Jinyu Zhang, Jingyi Liang, Xiaojun Huang, Shuang Zhang, Fei Lv, Zhusheng Guo","doi":"10.1002/rcm.70053","DOIUrl":"10.1002/rcm.70053","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Background</h3>\u0000 \u0000 <p>The rising incidence of Salmonella-induced diarrhea highlights the critical need for judicious antibiotic use to ensure effective treatment outcomes.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>This study presents an innovative methodology for evaluating the susceptibility of Salmonella to ceftriaxone and azithromycin through the application of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The proposed method requires only 2–3 individual Salmonella colonies and yields results within approximately 1 hour, assessing susceptibility to ceftriaxone (70 mg/L) and azithromycin (25 mg/L). In comparison to the Kirby-Bauer method, this technique exhibits a sensitivity of 98.64% and a specificity of 84.38%.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The method developed in this study is both straightforward and user-friendly, making it suitable for deployment in major laboratories equipped with time-of-flight mass spectrometry. It offers a preliminary assessment of Salmonella susceptibility to ceftriaxone and azithromycin, thereby enhancing the accuracy of clinical interventions for Salmonella infections.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146211785","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}
Odilon Leite-Barbosa, Marcelo Ferreira Leão de Oliveira, Márcia Gomes de Oliveira, Monica Costa Padilha, Valdir Florêncio Veiga-Junior
Rationale
The migration of phthalate plasticizers from high-volume polymers, such as poly(vinyl chloride) (PVC), raises significant toxicological concerns, particularly when materials are subjected to aging and environmental stress. As traditional monitoring techniques rely on time-consuming solvent extraction and chromatographic methods that are often expensive and lack the throughput required for large-scale safety screening, this study intends to present a rapid screening method using direct analysis in real time coupled to high-resolution mass spectrometry (DART-HRMS) to monitor plasticizer migration in PVC films subjected to accelerated UV aging. Operational parameters, such as ionization gas temperature and grid voltage, were systematically optimized to balance desorption efficiency with molecular integrity.
Methods
DART-HRMS analysis of three commercial PVC films subjected to accelerated UV aging (ASTM G154-23) was performed after optimization of the operational parameters: ionization gas temperature: 250 °C, 350 °C, and 500 °C and grid voltage: 50 and 350 V were systematically optimized to balance desorption efficiency with molecular integrity.
Results
Analytical performance was strongly governed by source energy, with optimal conditions achieved at 350 °C and 50 V, yielding the highest signal stability and minimal in-source fragmentation. Elevated grid voltage (350 V) caused severe signal suppression and fragmentation, particularly for high-molecular-weight plasticizers such as DIDP and DINP. Application of the optimized method revealed formulation-dependent migration behavior during UV aging. Short-chain phthalates showed rapid and, in some cases, transient surface enrichment, whereas medium- and high-molecular-weight plasticizers exhibited delayed or limited migration, becoming detectable only after prolonged exposure.
Conclusions
DART-HRMS provides a fast, robust, and solvent-free approach for screening plasticizer migration in PVC films. The optimized conditions enable sensitive detection while preserving molecular integrity, allowing differentiation of additive mobility as a function of molecular weight, formulation, and UV-induced degradation. This methodology offers a high-throughput alternative for assessing additive stability and potential release in consumer-grade PVC materials.
{"title":"Rapid Detection of Plasticizer Migration From UV-Aged PVC Films by DART-HRMS","authors":"Odilon Leite-Barbosa, Marcelo Ferreira Leão de Oliveira, Márcia Gomes de Oliveira, Monica Costa Padilha, Valdir Florêncio Veiga-Junior","doi":"10.1002/rcm.70048","DOIUrl":"10.1002/rcm.70048","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>The migration of phthalate plasticizers from high-volume polymers, such as poly(vinyl chloride) (PVC), raises significant toxicological concerns, particularly when materials are subjected to aging and environmental stress. As traditional monitoring techniques rely on time-consuming solvent extraction and chromatographic methods that are often expensive and lack the throughput required for large-scale safety screening, this study intends to present a rapid screening method using direct analysis in real time coupled to high-resolution mass spectrometry (DART-HRMS) to monitor plasticizer migration in PVC films subjected to accelerated UV aging. Operational parameters, such as ionization gas temperature and grid voltage, were systematically optimized to balance desorption efficiency with molecular integrity.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>DART-HRMS analysis of three commercial PVC films subjected to accelerated UV aging (ASTM G154-23) was performed after optimization of the operational parameters: ionization gas temperature: 250 °C, 350 °C, and 500 °C and grid voltage: 50 and 350 V were systematically optimized to balance desorption efficiency with molecular integrity.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Analytical performance was strongly governed by source energy, with optimal conditions achieved at 350 °C and 50 V, yielding the highest signal stability and minimal in-source fragmentation. Elevated grid voltage (350 V) caused severe signal suppression and fragmentation, particularly for high-molecular-weight plasticizers such as DIDP and DINP. Application of the optimized method revealed formulation-dependent migration behavior during UV aging. Short-chain phthalates showed rapid and, in some cases, transient surface enrichment, whereas medium- and high-molecular-weight plasticizers exhibited delayed or limited migration, becoming detectable only after prolonged exposure.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>DART-HRMS provides a fast, robust, and solvent-free approach for screening plasticizer migration in PVC films. The optimized conditions enable sensitive detection while preserving molecular integrity, allowing differentiation of additive mobility as a function of molecular weight, formulation, and UV-induced degradation. This methodology offers a high-throughput alternative for assessing additive stability and potential release in consumer-grade PVC materials.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12911472/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146211779","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}
Michael J. Mohr, Linus Strähle, Tobias Bader, Pia Leurle, Jan H. Christensen, Wolfram Seitz, Rudi Winzenbacher
Rationale
The quality of analytical measurements is typically evaluated after completion of the entire, or possibly multiple, measurement batch(es). Automated, near real-time quality control (QC) during LC-HRMS acquisition can prevent reruns and sample loss by flagging issues as they occur. Functionality was evaluated by retrospective application to 5 years of river-water surveillance.
Methods
We present a modular MATLAB workflow that tracks isotopically labelled internal standards for peak height, retention time and mass error against rolling, method-specific expectations; applies multivariate statistical process control (MSPC; PCA with Hotelling's T2 and SPE on intensity/retention time ratios and mass error); issues immediate email alerts; and logs outcomes to a PostgreSQL database/Grafana dashboard for trend analysis. Also, qualitative target screening via cosine-similarity MS2 checks against a local library, retention time correction, robust peak-height/noise estimation, configurable limits and automated vendor-to-open format conversion.
Results
In a high-voltage power-supply failure, 25/25 injections were flagged due to abnormal intensity patterns; during an organic-pump malfunction, 17/25 were flagged for retention drift up to and beyond the extraction window; and during an air-conditioning (AC) outage, MSPC detected mass error anomalies even when the ±10 ppm univariate limit was not breached. MSPC closely agreed with univariate thresholds: 95.7% of samples flagged by univariate rules were also flagged by MSPC (≈4.3% Type II), while 92.5% of MSPC-flagged samples violated at least one univariate rule (≈7.5% Type I).
Conclusion
These capabilities enable immediate detection, triage and documentation of performance excursions, support proactive maintenance (e.g., column aging or pump delivery issues), minimise downtime and safeguard precious samples. Although showcased on a specific LC-HRMS setup and matrix, the workflow is instrument-agnostic and broadly applicable to internal-standardised LC-HRMS methods.
{"title":"Automated Near Real-Time QC for LC-HRMS","authors":"Michael J. Mohr, Linus Strähle, Tobias Bader, Pia Leurle, Jan H. Christensen, Wolfram Seitz, Rudi Winzenbacher","doi":"10.1002/rcm.70052","DOIUrl":"10.1002/rcm.70052","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>The quality of analytical measurements is typically evaluated after completion of the entire, or possibly multiple, measurement batch(es). Automated, near real-time quality control (QC) during LC-HRMS acquisition can prevent reruns and sample loss by flagging issues as they occur. Functionality was evaluated by retrospective application to 5 years of river-water surveillance.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>We present a modular MATLAB workflow that tracks isotopically labelled internal standards for peak height, retention time and mass error against rolling, method-specific expectations; applies multivariate statistical process control (MSPC; PCA with Hotelling's <i>T</i><sup>2</sup> and SPE on intensity/retention time ratios and mass error); issues immediate email alerts; and logs outcomes to a PostgreSQL database/Grafana dashboard for trend analysis. Also, qualitative target screening via cosine-similarity MS<sup>2</sup> checks against a local library, retention time correction, robust peak-height/noise estimation, configurable limits and automated vendor-to-open format conversion.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>In a high-voltage power-supply failure, 25/25 injections were flagged due to abnormal intensity patterns; during an organic-pump malfunction, 17/25 were flagged for retention drift up to and beyond the extraction window; and during an air-conditioning (AC) outage, MSPC detected mass error anomalies even when the ±10 ppm univariate limit was not breached. MSPC closely agreed with univariate thresholds: 95.7% of samples flagged by univariate rules were also flagged by MSPC (≈4.3% Type II), while 92.5% of MSPC-flagged samples violated at least one univariate rule (≈7.5% Type I).</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>These capabilities enable immediate detection, triage and documentation of performance excursions, support proactive maintenance (e.g., column aging or pump delivery issues), minimise downtime and safeguard precious samples. Although showcased on a specific LC-HRMS setup and matrix, the workflow is instrument-agnostic and broadly applicable to internal-standardised LC-HRMS methods.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12933221/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146211741","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}
François Fourel, Christophe Lécuyer, Emilie Thomassot, Etienne Deloule, Charles Ojeimi
Rationale
Diamonds are generally considered to be metasomatic minerals originating from the Earth's mantle. They formed through the interaction of carbon-bearing fluids or melts with the surrounding deep lithology. Most knowledge about the formation of diamonds comes from studying their mineral inclusions or stable isotopes. Furthermore, diamonds are the only geological samples that provide insight into the volatile element composition of the Earth's mantle. While hydrogen has been known since the early 1970s to be a common impurity in natural diamonds, only a few studies have provided satisfactory quantitative measurements of its concentration and isotopic composition.
Methods
Here, we compare the results obtained using two different techniques involving EA-IRMS. The first analytical procedure involves H-pyrolysis and is a modification from existing techniques. The second innovative setup, which has not yet been described, involves diamond combustion followed by hydrogen reduction.
Results
As diamond test samples are rare, we first analysed analogous samples (graphite) to validate the method, before analysing polycrystalline diamonds (from the Orapa mine in Botswana) with both techniques. After assessing the consistency between the two procedures, we analysed three natural diamonds. The results obtained using both techniques were highly comparable. This confirmed the validity of the H-Pyrolysis method, which is slightly more sensitive.
Conclusions
We designed and validated a novel methodology to incorporate an additional isotopic record into diamonds, namely, carbon, oxygen and nitrogen, with the objective of tracing the formation process of natural diamonds. Diamond in situ analyses might enhance our comprehension of the deep water cycle. Those measurements require precisely calibrated materials. This technique could provide such references.
{"title":"Combustion and Pyrolysis EA-IRMS Techniques to Determine the δ2H of Diamonds","authors":"François Fourel, Christophe Lécuyer, Emilie Thomassot, Etienne Deloule, Charles Ojeimi","doi":"10.1002/rcm.70041","DOIUrl":"10.1002/rcm.70041","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Diamonds are generally considered to be metasomatic minerals originating from the Earth's mantle. They formed through the interaction of carbon-bearing fluids or melts with the surrounding deep lithology. Most knowledge about the formation of diamonds comes from studying their mineral inclusions or stable isotopes. Furthermore, diamonds are the only geological samples that provide insight into the volatile element composition of the Earth's mantle. While hydrogen has been known since the early 1970s to be a common impurity in natural diamonds, only a few studies have provided satisfactory quantitative measurements of its concentration and isotopic composition.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Here, we compare the results obtained using two different techniques involving EA-IRMS. The first analytical procedure involves H-pyrolysis and is a modification from existing techniques. The second innovative setup, which has not yet been described, involves diamond combustion followed by hydrogen reduction.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>As diamond test samples are rare, we first analysed analogous samples (graphite) to validate the method, before analysing polycrystalline diamonds (from the Orapa mine in Botswana) with both techniques. After assessing the consistency between the two procedures, we analysed three natural diamonds. The results obtained using both techniques were highly comparable. This confirmed the validity of the H-Pyrolysis method, which is slightly more sensitive.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>We designed and validated a novel methodology to incorporate an additional isotopic record into diamonds, namely, carbon, oxygen and nitrogen, with the objective of tracing the formation process of natural diamonds. Diamond in situ analyses might enhance our comprehension of the deep water cycle. Those measurements require precisely calibrated materials. This technique could provide such references.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12906137/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146193842","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}
Daniel S. McCracken, David J. Foreman, Kyle G. Esposito, Alyssa Q. Stiving, Benjamin W. Roose, Danielle V. Miller, Feras Hatahet
Background
Tris(2-carboxyethyl)phosphine (TCEP) is a commonly used laboratory reagent for the purposes of reducing disulfide bonds. TCEP is often preferred over alternative reducing reagents, such as dithiothreitol (DTT), due to its strong redox potential, effectiveness in a broad pH range, and handling considerations. Despite this, many side reactions involving TCEP have been poorly categorized and understood.
Finding
Utilizing a combination of gel electrophoresis and mass spectrometry techniques, we have discovered a unique and novel mechanism by which TCEP engages in the hydrolysis of proteins. This behavior has been observed to be site specific to the carboxyl terminus of aspartic acid residues.
Conclusion
Cleavage at this location is completely independent of the reduction of disulfide bonds in proteins due to the observance of this phenomenon in proteins lacking disulfide bonds, and some lacking cysteines altogether. While the specific chemistry of this hydrolysis is unknown, this discovery has potentially wide-ranging impacts as a sample preparation tool for mass spectrometry analysis, as well as being cautionary towards other common laboratory uses of this ubiquitous reagent where it could potentially cause unwanted hydrolysis of proteins being studied.
Impact
The broader analytical implications of this finding are that many previously unknown origin artifacts can now be properly attributed to a source, particularly in areas such as proteomic sample preparation, redox chemistries studies, and similar. This also expands our knowledge of TCEP chemistry beyond simply a disulfide bond reductor, offering both methodological opportunities for peptide mapping and important cautionary implications for biochemical sample treatment.
{"title":"TCEP-Mediated Protein Hydrolysis: Highly Selective Cleavage C-Terminal to Aspartic Acid","authors":"Daniel S. McCracken, David J. Foreman, Kyle G. Esposito, Alyssa Q. Stiving, Benjamin W. Roose, Danielle V. Miller, Feras Hatahet","doi":"10.1002/rcm.70051","DOIUrl":"10.1002/rcm.70051","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Background</h3>\u0000 \u0000 <p>Tris(2-carboxyethyl)phosphine (TCEP) is a commonly used laboratory reagent for the purposes of reducing disulfide bonds. TCEP is often preferred over alternative reducing reagents, such as dithiothreitol (DTT), due to its strong redox potential, effectiveness in a broad pH range, and handling considerations. Despite this, many side reactions involving TCEP have been poorly categorized and understood.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Finding</h3>\u0000 \u0000 <p>Utilizing a combination of gel electrophoresis and mass spectrometry techniques, we have discovered a unique and novel mechanism by which TCEP engages in the hydrolysis of proteins. This behavior has been observed to be site specific to the carboxyl terminus of aspartic acid residues.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>Cleavage at this location is completely independent of the reduction of disulfide bonds in proteins due to the observance of this phenomenon in proteins lacking disulfide bonds, and some lacking cysteines altogether. While the specific chemistry of this hydrolysis is unknown, this discovery has potentially wide-ranging impacts as a sample preparation tool for mass spectrometry analysis, as well as being cautionary towards other common laboratory uses of this ubiquitous reagent where it could potentially cause unwanted hydrolysis of proteins being studied.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Impact</h3>\u0000 \u0000 <p>The broader analytical implications of this finding are that many previously unknown origin artifacts can now be properly attributed to a source, particularly in areas such as proteomic sample preparation, redox chemistries studies, and similar. This also expands our knowledge of TCEP chemistry beyond simply a disulfide bond reductor, offering both methodological opportunities for peptide mapping and important cautionary implications for biochemical sample treatment.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 10","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146193839","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}
Stems of Bauhinia championii (Benth.) Benth (Longxuteng in Chinese, LXT) are widely used folkloric traditional medicine in China, which is mainly utilized to treat rheumatoid arthritis, epigastric pain, and traumatic injury. Nevertheless, the comprehensive components correlated to the therapeutic efficacy are still unclear. Our study aims to characterize constituents in LXT extract and their metabolites in plasma and subsequently provide detailed compositional information for the LXT's quality evaluation and mechanism researches.
Methods
Ultraperformance Liquid Chromatography–Orbitrap Elite Combined High Resolution Mass Spectrometer (UPLC-LTQ/Orbitrap HRMS) was used to identify the constituents of LXT and their metabolites in plasma. The HRMS data were analyzed by Xcalibur, and the constituents were identified by the MS2 profile, characteristic fragments, and cleavage patterns by comparative analysis using authentic standards, online mass spectral libraries, and literature reports.
Results
Forty-six components in LXT extract were identified, including 28 flavonoids, 5 phenylpropanoids, 10 organic acids, 1 carbohydrate, 1 nucleoside, and 1 alkaloid. Among them, 27 components were detected from LXT for the first time. Meanwhile, 54 compounds were found in plasma, including 11 prototypes and 43 metabolites. The prototypes, which are mainly polymethoxyflavones, dihydroflavonol glycosides, and flavanols, seem to be potential pharmacodynamic components of LXT.
Conclusion
This is the first report on the comprehensive component identification of LXT extract and its metabolites in plasma by using LC-MS. Our findings may serve as a theoretical basis for LXT's quality evaluation and mechanism research.
{"title":"Characterization of the Constituents of the Stem of Bauhinia championii (Benth.) Benth and Their Metabolites in Rat Plasma by UPLC-LTQ/Orbitrap HRMS","authors":"Shiren Deng, Hao Yang, Xiaoxia Chen, Linbo Xia","doi":"10.1002/rcm.70045","DOIUrl":"10.1002/rcm.70045","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Stems of <i>Bauhinia championii</i> (Benth.) Benth (Longxuteng in Chinese, LXT) are widely used folkloric traditional medicine in China, which is mainly utilized to treat rheumatoid arthritis, epigastric pain, and traumatic injury. Nevertheless, the comprehensive components correlated to the therapeutic efficacy are still unclear. Our study aims to characterize constituents in LXT extract and their metabolites in plasma and subsequently provide detailed compositional information for the LXT's quality evaluation and mechanism researches.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Ultraperformance Liquid Chromatography–Orbitrap Elite Combined High Resolution Mass Spectrometer (UPLC-LTQ/Orbitrap HRMS) was used to identify the constituents of LXT and their metabolites in plasma. The HRMS data were analyzed by Xcalibur, and the constituents were identified by the MS<sup>2</sup> profile, characteristic fragments, and cleavage patterns by comparative analysis using authentic standards, online mass spectral libraries, and literature reports.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Forty-six components in LXT extract were identified, including 28 flavonoids, 5 phenylpropanoids, 10 organic acids, 1 carbohydrate, 1 nucleoside, and 1 alkaloid. Among them, 27 components were detected from LXT for the first time. Meanwhile, 54 compounds were found in plasma, including 11 prototypes and 43 metabolites. The prototypes, which are mainly polymethoxyflavones, dihydroflavonol glycosides, and flavanols, seem to be potential pharmacodynamic components of LXT.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>This is the first report on the comprehensive component identification of LXT extract and its metabolites in plasma by using LC-MS. Our findings may serve as a theoretical basis for LXT's quality evaluation and mechanism research.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 9","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146130476","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}
Alan M. Rowland, Stephen E. Smith, Ella F. Vandergriff, Arturo Rodriguez, David P. Lewis, Kevin P. Schultze, William M. Gilliland Jr.
With the goal of sensitive, selective, targeted, and portable VOC quantification, an atmospheric pressure photoionization (APPI) source was developed for a miniature high pressure mass spectrometer, the MX908. The APPI source consists of a VUV lamp that was encased in a custom 3D-printed apparatus. Using m-xylene as the testing standard, the effects of pressure, axial RF voltage, aperture voltage, and humidity on the instrument were investigated and optimized. Operating at 0.8 Torr with ambient air as the buffer gas, the instrument showed linearity from 25 to 500 ppbV for benzene, toluene, ethylbenzene, and m-xylene without preconcentration.
{"title":"Development of an Atmospheric-Pressure Photoionization Source for VOC Detection With a Miniature High-Pressure Mass Spectrometer","authors":"Alan M. Rowland, Stephen E. Smith, Ella F. Vandergriff, Arturo Rodriguez, David P. Lewis, Kevin P. Schultze, William M. Gilliland Jr.","doi":"10.1002/rcm.70050","DOIUrl":"10.1002/rcm.70050","url":null,"abstract":"<p>With the goal of sensitive, selective, targeted, and portable VOC quantification, an atmospheric pressure photoionization (APPI) source was developed for a miniature high pressure mass spectrometer, the MX908. The APPI source consists of a VUV lamp that was encased in a custom 3D-printed apparatus. Using <i>m</i>-xylene as the testing standard, the effects of pressure, axial RF voltage, aperture voltage, and humidity on the instrument were investigated and optimized. Operating at 0.8 Torr with ambient air as the buffer gas, the instrument showed linearity from 25 to 500 ppbV for benzene, toluene, ethylbenzene, and <i>m</i>-xylene without preconcentration.</p>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 9","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12875154/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146111603","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}
Amoxicillin is a broad-spectrum β-lactam antibiotic that is prone to undergo degradation under various stress and storage conditions into multiple impurities, which may compromise drug stability, efficacy, and safety. This study established an eco-efficient comprehensive analytical strategy for amoxicillin degradation impurities using UHPLC coupled with PDA detection and QTOF-MS characterization, which has not been previously reported.
Methods
Chromatographic conditions were optimized through software-assisted conversion from traditional chromatography and then validated for the simultaneous determination of degradation impurities. Separation was performed on a Cortecs C18 column (150 × 3 mm; 2.7 μm) at 254 nm with a gradient elution of acetonitrile and a pH 5.0 buffer solution. Degradation products were identified and characterized using UHPLC-PDA/Q/TOF-MS. The environmental impact of the method was evaluated using the Eco-Scale, GAPI, AGREE, and BAGI tools.
Results
The validated method in accordance with ICH Q2(R2) (2023) demonstrates system suitability, specificity, linearity (3.003–22.519 μg/mL), accuracy (98.0%–102%, RSD < 2.0%), precision (RSD < 2.0%), and robustness. Limits of detection and quantification were 0.330 and 0.991 μg/mL, respectively, enabling the quantification of impurities at 0.066% relative to amoxicillin content in 500-mg capsules. Four degradation impurities exceeding the identification thresholds were characterized, including amoxicillin diketopiperazine, penilloic acid, and two newly detected compounds not listed in the current international pharmacopoeias. Greenness evaluation tools confirm the environmental friendliness of the method, with high scores of 78 (Eco-Scale), 80 (BAGI), 68 (GAPI), and 0.63 (AGREE).
Conclusions
The study delivers enhanced chromatographic resolution for understanding the degradation pathways of amoxicillin during short- and long-term storage, enabling stability evaluation and routine drug quality control in accordance with sustainable development goals.
{"title":"A Sustainable UHPLC-PDA/QTOF-MS Approach for Comprehensive Profiling of Amoxicillin Degradation Impurities","authors":"Vo Thi Kim Khuyen, Do Thanh Nhu, Nguyen Duc Tuan","doi":"10.1002/rcm.70046","DOIUrl":"10.1002/rcm.70046","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Amoxicillin is a broad-spectrum β-lactam antibiotic that is prone to undergo degradation under various stress and storage conditions into multiple impurities, which may compromise drug stability, efficacy, and safety. This study established an eco-efficient comprehensive analytical strategy for amoxicillin degradation impurities using UHPLC coupled with PDA detection and QTOF-MS characterization, which has not been previously reported.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Chromatographic conditions were optimized through software-assisted conversion from traditional chromatography and then validated for the simultaneous determination of degradation impurities. Separation was performed on a Cortecs C18 column (150 × 3 mm; 2.7 μm) at 254 nm with a gradient elution of acetonitrile and a pH 5.0 buffer solution. Degradation products were identified and characterized using UHPLC-PDA/Q/TOF-MS. The environmental impact of the method was evaluated using the Eco-Scale, GAPI, AGREE, and BAGI tools.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The validated method in accordance with ICH Q2(R2) (2023) demonstrates system suitability, specificity, linearity (3.003–22.519 μg/mL), accuracy (98.0%–102%, RSD < 2.0%), precision (RSD < 2.0%), and robustness. Limits of detection and quantification were 0.330 and 0.991 μg/mL, respectively, enabling the quantification of impurities at 0.066% relative to amoxicillin content in 500-mg capsules. Four degradation impurities exceeding the identification thresholds were characterized, including amoxicillin diketopiperazine, penilloic acid, and two newly detected compounds not listed in the current international pharmacopoeias. Greenness evaluation tools confirm the environmental friendliness of the method, with high scores of 78 (Eco-Scale), 80 (BAGI), 68 (GAPI), and 0.63 (AGREE).</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The study delivers enhanced chromatographic resolution for understanding the degradation pathways of amoxicillin during short- and long-term storage, enabling stability evaluation and routine drug quality control in accordance with sustainable development goals.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 9","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146099710","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}
Isaure Sergent, Ian Roszak, Jean-François Lutz, Laurence Charles
Rationale
MS/MS sequencing is commonly used to read binary messages encoded in digital polymers. To achieve full sequence coverage required for error-free reading, the structure of coding units is usually optimized to prevent extensive signal dilution over multiple fragmentation routes. Changing ionization polarity can also have a significant effect on MS/MS pattern, which is explored here for poly(amino phosphodiester)s.
Methods
Poly(amino phosphodiester)s (N-PPDEs) include comonomers composed of one phosphate group and a main-chain tertiary amine holding different alkyl substituents as coding moieties. Accordingly, they can be readily ionized in both polarity modes, using ammonium acetate to promote electrospray formation of deprotonated species and protonated molecules when switching from negative to positive ion mode. Changes of their MS/MS spectra are studied with regard to the behavior of their PPDE homologues lacking the main-chain tertiary amine.
Results
In collision-induced dissociation (CID) conditions, eight fragment series are produced upon cleavage of all phosphate bonds in deprotonated species, whereas only four ion series are generated from protonated N-PPDEs in which O–P–O linkages remain intact. The advantageous MS/MS behavior of protonated N-PPDEs has been rationalized by considering that protons located on tertiary amines are also solvated by nearby phosphate groups, promoting exclusive cleavage of C–O bonds.
Conclusions
In contrast to PPDEs, switching from deprotonated to protonated precursors yields highly simplified CID data for N-PPDEs, opening promising perspectives for reliable MS/MS sequencing of long coded polymers.
{"title":"Switching Ionization Polarity to Simplify MS/MS Sequencing of Digital Polymers: the Case of Informational Poly(Amino phosphodiester)s","authors":"Isaure Sergent, Ian Roszak, Jean-François Lutz, Laurence Charles","doi":"10.1002/rcm.70047","DOIUrl":"10.1002/rcm.70047","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>MS/MS sequencing is commonly used to read binary messages encoded in digital polymers. To achieve full sequence coverage required for error-free reading, the structure of coding units is usually optimized to prevent extensive signal dilution over multiple fragmentation routes. Changing ionization polarity can also have a significant effect on MS/MS pattern, which is explored here for poly(amino phosphodiester)s.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Poly(amino phosphodiester)s (N-PPDEs) include comonomers composed of one phosphate group and a main-chain tertiary amine holding different alkyl substituents as coding moieties. Accordingly, they can be readily ionized in both polarity modes, using ammonium acetate to promote electrospray formation of deprotonated species and protonated molecules when switching from negative to positive ion mode. Changes of their MS/MS spectra are studied with regard to the behavior of their PPDE homologues lacking the main-chain tertiary amine.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>In collision-induced dissociation (CID) conditions, eight fragment series are produced upon cleavage of all phosphate bonds in deprotonated species, whereas only four ion series are generated from protonated N-PPDEs in which O–P–O linkages remain intact. The advantageous MS/MS behavior of protonated N-PPDEs has been rationalized by considering that protons located on tertiary amines are also solvated by nearby phosphate groups, promoting exclusive cleavage of C–O bonds.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>In contrast to PPDEs, switching from deprotonated to protonated precursors yields highly simplified CID data for N-PPDEs, opening promising perspectives for reliable MS/MS sequencing of long coded polymers.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 9","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12861711/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146099746","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}
Bushen Huoxue (BSHX) decoction is effective against intervertebral disc degeneration (IVDD) and osteoarthritis, but its mechanism remains unclear. This study investigates its potential role in regulating efferocytosis in IVDD.
Methods
BSHX decoction, prepared from Eucommia ulmoides, Psoralea corylifolia, Achyranthes bidentata, Salvia miltiorrhiza, Clematis chinensis, and Chaenomeles speciosa, was extracted, concentrated, and analyzed by LC–MS/MS to identify active ingredients. Swiss TargetPrediction analysis predicted all targets. The PPI network was constructed using STRING 12.0 and CytoNCA in Cytoscape, followed by GO and KEGG enrichment analyses. Three publicly available datasets (GSE70362, GSE124272, GSE150408) were analyzed for differential gene expression in IVDD, with efferocytosis-related genes retrieved from GeneCards and KEGG, and candidate targets identified by intersecting PPI network core targets with efferocytosis-related differentially expressed genes (EFRDEGs). A network pharmacology model was then constructed, followed by molecular docking, molecular dynamics simulations, and pharmacokinetic properties.
Results
A total of 77 active ingredients and 298 targets were identified, with ELANE, MPO, and RXRA selected as candidate targets through bioinformatics analysis. GO and KEGG analyses highlighted their roles in immune regulation, inflammation, apoptosis, and tissue repair. Network analysis suggests that these compounds regulate multiple pathways, providing a mechanism for BSHX decoction to alleviate IVDD by modulating efferocytosis. Molecular docking showed strong binding affinity (binding energy < −8.0 kcal/mol) of tanshinone II A, pinoresinol diglucoside, and psoralidin with ELANE, MPO, and RXRA. Molecular dynamics simulation of the MPO–pinoresinol diglucoside complex confirmed its stability, and we revealed that pinoresinol diglucoside possesses favorable pharmacokinetic properties and safety characteristics.
Conclusion
BSHX decoction may exert therapeutic effects on IVDD by targeting ELANE, MPO, and RXRA to regulate multiple pathways involved in efferocytosis. These findings offer valuable insights into the underlying mechanisms of BSHX decoction in the treatment of IVDD, providing a solid theoretical basis for the clinical application of traditional Chinese medicine.
{"title":"Exploring the Mechanistic Role of Bushen Huoxue Decoction in Treating Intervertebral Disc Degeneration Through Efferocytosis Regulation","authors":"Hongtao Li, Changxiao Han, Jiacheng Zheng, Zhiwen Li, Xu Wang, Liguo Zhu, Minshan Feng","doi":"10.1002/rcm.70043","DOIUrl":"10.1002/rcm.70043","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Background</h3>\u0000 \u0000 <p>Bushen Huoxue (BSHX) decoction is effective against intervertebral disc degeneration (IVDD) and osteoarthritis, but its mechanism remains unclear. This study investigates its potential role in regulating efferocytosis in IVDD.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>BSHX decoction, prepared from <i>Eucommia ulmoides</i>, <i>Psoralea corylifolia</i>, <i>Achyranthes bidentata</i>, <i>Salvia miltiorrhiza</i>, Clematis chinensis, and <i>Chaenomeles speciosa</i>, was extracted, concentrated, and analyzed by LC–MS/MS to identify active ingredients. Swiss TargetPrediction analysis predicted all targets. The PPI network was constructed using STRING 12.0 and CytoNCA in Cytoscape, followed by GO and KEGG enrichment analyses. Three publicly available datasets (GSE70362, GSE124272, GSE150408) were analyzed for differential gene expression in IVDD, with efferocytosis-related genes retrieved from GeneCards and KEGG, and candidate targets identified by intersecting PPI network core targets with efferocytosis-related differentially expressed genes (EFRDEGs). A network pharmacology model was then constructed, followed by molecular docking, molecular dynamics simulations, and pharmacokinetic properties.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>A total of 77 active ingredients and 298 targets were identified, with ELANE, MPO, and RXRA selected as candidate targets through bioinformatics analysis. GO and KEGG analyses highlighted their roles in immune regulation, inflammation, apoptosis, and tissue repair. Network analysis suggests that these compounds regulate multiple pathways, providing a mechanism for BSHX decoction to alleviate IVDD by modulating efferocytosis. Molecular docking showed strong binding affinity (binding energy < −8.0 kcal/mol) of tanshinone II A, pinoresinol diglucoside, and psoralidin with ELANE, MPO, and RXRA. Molecular dynamics simulation of the MPO–pinoresinol diglucoside complex confirmed its stability, and we revealed that pinoresinol diglucoside possesses favorable pharmacokinetic properties and safety characteristics.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>BSHX decoction may exert therapeutic effects on IVDD by targeting ELANE, MPO, and RXRA to regulate multiple pathways involved in efferocytosis. These findings offer valuable insights into the underlying mechanisms of BSHX decoction in the treatment of IVDD, providing a solid theoretical basis for the clinical application of traditional Chinese medicine.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 9","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146083666","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}
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