Rapid Communications in Mass Spectrometry最新文献

{"title":"Part A: Implementing an Analyte Panel and Sampling Protocol for Quality Control in Mass Spectrometry Imaging","authors":"Quinn Mills,&nbsp;Russell R. Kibbe,&nbsp;Alexandria L. Sohn,&nbsp;Andrew J. Percy,&nbsp;Krista Backiel,&nbsp;David C. Muddiman","doi":"10.1002/rcm.9993","DOIUrl":"https://doi.org/10.1002/rcm.9993","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>While quality control (QC) and system suitability testing (SST) methods are commonly employed in mass spectrometry, the field of mass spectrometry imaging (MSI) currently lacks any universally accepted QC/SST protocols. These methods can prevent the loss of precious samples due to suboptimal instrument conditions and/or data quality, but they are more challenging to implement on MSI platforms. Herein, a panel of analytes is conveniently analyzed in a setup that reflects a typical MSI imaging experiment, and guidance is provided for downstream QC/SST evaluation.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>The analyte panel will be commercially available and consists of three pairs of unlabeled (NAT) analytes and their stable isotope–labeled (SIL) analogues; a deviation from the standard procedure is also included, which incorporates a polymer to expand <i>m</i>/<i>z</i> coverage. The NAT three-plex (or four-plex with the added polymer) is analyzed as a droplet on a slide, and the SIL three-plex is doped into the electrospray solvent, isolating the NAT and SIL compounds to different source components. Datasets are collected on clean and compromised instruments to inform QC/SST software and later evaluate instrument conditions or isolated metrics of data quality.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>A procedure was created for QC/SST analysis on MSI platforms, which can be optionally paired with the freely available software Supervised Learning for Instrument Classification and Evaluation for Mass Spectrometry Imaging (SLICE-MSI) to classify the condition of the instrument. The SIL data may be monitored separately during imaging experiments for continuous evaluation of electrospray stability. The protocol highlights areas that may be adapted for other ionization sources for widespread use.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The protocol described herein uses a panel of NAT and SIL compounds to offer an objective and accurate determination of QC/SST on MSI platforms.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.9993","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143431445","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":"Improved Protective Effects and Pharmacokinetics of Huperzine A Derivative H14 in Soman Poisoning: A Comparative Study With Huperzine A in Rats","authors":"Guixiang Yang,&nbsp;Yalan Cui,&nbsp;Xingxing Zong,&nbsp;Qian Jin,&nbsp;Yi Zhang,&nbsp;Liqin Li,&nbsp;Dongxin Liu,&nbsp;Xuejun Chen,&nbsp;Chen Wang,&nbsp;Jingchen Wei","doi":"10.1002/rcm.9995","DOIUrl":"https://doi.org/10.1002/rcm.9995","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p><i>N</i>-[2-Hydroxy-3,5-dimethylbenzilidene]-Hup A (H14) is a derivative of huperzine A (Hup A) that demonstrates superior protective effects against soman (GD) compared to Hup A. This study aims to evaluate the protective efficacy of H14 pretreatment against GD in rats and to provide an analytical framework for the pharmacokinetic evaluation of H14 in experimental animals.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>The study employed protective ratios (PR) as an evaluation criterion to assess the efficacy of H14 and Hup A in preventing GD in vivo. Liquid–liquid extraction techniques were utilized to extract H14 and its metabolite, Hup A, from plasma. The extracted plasma samples were then analyzed using an ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method for the simultaneous quantification of H14 and Hup A.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The PR values for the 6- and 12-h Hup A groups were 1.26 and 1.08, respectively. In contrast, the 6, 12, and 24-h H14 groups demonstrated PR values of 2.81, 1.98, and 1.18, respectively, indicating extended protective capabilities compared to Hup A. All validation parameters for the UHPLC–MS/MS method, including linearity, specificity, precision, accuracy, matrix effect, and stability, met the acceptance criteria established by FDA guidelines. The pharmacokinetic analysis indicates that H14, after conversion to Hup A in vivo, significantly extends the duration of Hup A concentrations in the body, leading to more effective prevention of GD poisoning compared to Hup A alone.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>H14 demonstrates superior efficacy in preventing GD poisoning compared to Hup A. Furthermore, this analytical approach offers a reliable and efficient method for the pharmacokinetic evaluation of H14 in experimental animals.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143424060","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":"Covalent Organic Framework Nanofilm-Assisted Laser Desorption Ionization Mass Spectrometry for the Determination of Benzophenone Derivatives in Personal Care Products","authors":"Ling Yan,&nbsp;Wenjun Zheng,&nbsp;Zian Lin","doi":"10.1002/rcm.10009","DOIUrl":"https://doi.org/10.1002/rcm.10009","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rational</h3>\u0000 \u0000 <p>Benzophenone derivatives, commonly used as UV filters in personal care products (PCPs), are widely prevalent and raise concerns due to their endocrine-disrupting effects. Sensitive and efficient analytical methods are in demand for their detection. In this study, we developed a TAPB-DMTP-covalent organic framework (COF) nanofilm-assisted laser desorption ionization mass spectrometry (LDI-MS) method for the quantitative analysis of 2,4-dihydroxybenzophenone (BP-1) in PCPs.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>The TAPB-DMTP-COF nanofilm was synthesized on indium tin oxide (ITO) glass and utilized as an LDI-MS substrate. The performance of TAPB-DMTP-COF nanofilm-assisted LDI-MS for analyzing small molecules (e.g., benzophenone derivatives, phthalates, amino acids, sugars, and nucleosides) was compared to conventional organic matrices (α-cyano-4-hydroxycinnamic acid [CHCA], 2,5-dihydroxybenzoic acid [DHB], and sinapinic acid [SA]). The reproducibility, salt resistance, sensitivity, and stability of the method were further evaluated. Finally, the technique was applied to quantify BP-1 in PCPs.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The TAPB-DMTP-COF nanofilm-assisted LDI-MS provided stronger mass spectral signals and cleaner backgrounds for small molecules compared to CHCA, DHB, and SA. The method exhibited high reproducibility (RSD = 6.10%) and stability for up to 30 days. BP-1 in PCPs was quantified with excellent linearity (1–20 μg/mL, <i>r</i> = 0.9993), a low detection limit (0.3 μg/mL), and recovery rates of 94.2%–104.4%, demonstrating the potential of TAPB-DMTP-COF nanofilm for sensitive and reliable small-molecule analysis.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>TAPB-DMTP-COF nanofilm-assisted LDI-MS offered the advantages of rapid analysis, clean backgrounds, and reproducibility for detecting small molecules, including benzophenone derivatives. This method successfully quantified BP-1 in PCPs, highlighting its suitability for analyzing complex samples.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 10","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143404498","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":"Assessing Matrix and Nonmatrix, Single, and Multipoint Calibration of Trace Elements Using LA-ICP-MS on a Tropical Speleothem","authors":"Natasha Sekhon,&nbsp;Annabelle Gao,&nbsp;Soumen Mallick,&nbsp;Judson W. Partin,&nbsp;M. Bayani Cardenas,&nbsp;Daniel E. Ibarra","doi":"10.1002/rcm.9983","DOIUrl":"https://doi.org/10.1002/rcm.9983","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Suites of trace elements are routinely used in speleothems as proxies to understand periods of past climate change. Laser ablation techniques are regularly implemented to acquire high resolution (50-μm) trace element concentrations in carbonate archives for paleoclimatology. There exists limited research investigating Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) protocols using speleothem samples. This study investigates the difference between using matrix (carbonate) and nonmatrix (silicate) matched reference materials and the utility of 1-point versus multiple point calibration curves.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Following an extensive review of published literature on speleothem LA-ICP-MS analyses, we conducted two laser ablation experimental runs 8 months apart on a 2.7-cm section of a natural speleothem using matrix and nonmatrix matched reference materials. We used a 193-nm wavelength Analyte G2 laser attached to a X-Series-2 ICP-MS, a silicate reference material, and three carbonate reference materials. Next, we calculated concentrations using a 1-point calibration curve, a 2-point calibration curve, and a 3-point calibration curve.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The analysis of matrix and nonmatrix matched reference materials demonstrates that the trends of trace elements/Ca are minimally impacted by the matrix material of the standard. We also show that 2- and 3-point calibration curves bracket the range of sample concentrations compared to a 1-point (silicate) calibration curve. The calculated cave-air temperatures using Mg/Ca concentrations fall within error of each other regardless of the calibration curve approach applied.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Our experiments provide a proof of concept on the conventional setup of standards during LA-ICP-MS speleothem analysis. We suggest the use of at minimum a 2-point (silicate plus carbonate or carbonates) calibration curve that crucially bracket the range of sample concentrations rather than relying on a 1-point silicate standard that does not bracket the sample concentration. Finally, our results have implications for both speleothem studies that use LA-ICP-MS analytical techniques and additional carbonate archives.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143380818","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 Active Substances and Its Potential Mechanism of Gancao Fuzi Decoction on Inflammatory Based on Metabolomics and Network Pharmacology","authors":"Wei Geng,&nbsp;Shuang Liu,&nbsp;Hongjing Dong,&nbsp;Buddhika Niroshie Perumpuli Arachchige,&nbsp;Dongmei Qi,&nbsp;Xiao Wang","doi":"10.1002/rcm.10007","DOIUrl":"https://doi.org/10.1002/rcm.10007","url":null,"abstract":"<div>\u0000 \u0000 <p>Gancao Fuzi decoction (GCFZT) is a traditional Chinese formula, which has been commonly used in clinical practice to treat inflammatory diseases. However, the active substance of GCFZT in the treatment of inflammation is not fully clarified. In this study, we used orthogonal experiments to design different GCFZT formulations, resulting in a total of 16 GCFZT formulations. Subsequently, UPLC-Q-TOF-MS/MS was used to analyze the chemical composition of different formulations, and the anti-inflammatory activity differences of these formulations were evaluated through an LPS-induced RAW264.7 inflammatory cell model. Combined with machine learning algorithms such as PLS-DA and RF, four main active substances in GCFZT were screened. Finally, network pharmacology techniques were used to investigate the potential anti-inflammatory mechanisms of these main active substances, and the results showed that GCFZT mainly regulates the expression of core targets such as ALOX5, NFKB1, and TLR4 through main active substances such as chlorogenic acid, riboflavin, and formononetin, thereby affecting the NF kappa B signaling pathway, the Toll-like receptor signaling pathway, and the Th17 cell differentiation. This study provides a reference for the anti-inflammatory mechanism of GCFZT and a scientific basis for its clinical application.</p>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 10","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143380278","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":"Molecular Structure and Mass Spectral Data Quality-Driven Processing of High-Resolution Mass Spectrometry for Quantitative Analysis.","authors":"Fabien Fontaine, Luca Morettoni, Ken Anderson, Bernard Choi, Ismael Zamora, Kevin P Bateman","doi":"10.1002/rcm.10000","DOIUrl":"https://doi.org/10.1002/rcm.10000","url":null,"abstract":"<p><strong>Rationale: </strong>LC-MS-based quantification is traditionally performed using selected or multiple reaction monitoring (SRM/MRM) acquisition functions on triple quadrupole (QQQ) instruments resulting in both high sensitivity and selectivity. This workflow requires a previously identified reaction or transition from a precursor ion to a fragment ion to be monitored to obtain the needed selectivity for the compound of interest. High-resolution mass spectrometry (HRMS) has long sought to be a viable alternative for quantitatipve workflows but has been unable to broadly compete, mainly due to the lack of suitable data processing software.</p><p><strong>Methods: </strong>The approach we developed agnostically and automatically identifies all ions related to the compound being analyzed in both the MS and MSMS data, acquired with data-dependent or data-independent methods. The algorithm automatically selects optimal parameters (ion extraction window, ions to sum, etc.) to provide the best overall method to meet the acceptance criteria defined by the user (accuracy/precision).</p><p><strong>Results: </strong>The results obtained are directly compared to QQQ data collected from the same set of samples and show that the automated HRMS approach is as good as and, in some cases, better than the traditional QQQ approach in terms of selectivity, sensitivity, and dynamic range.</p><p><strong>Conclusions: </strong>This new methodology enables the use of generic methods for data collection for quantitative analysis using high-resolution mass spectrometry. With this approach, data collection is faster, and the processing algorithm provides quality equal to or better than the current QQQ methodology. This enables an overall reduction in cycle time and improved assay performance versus current HRMS-based quantitative analysis as well as traditional QQQ workflows.</p>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":" ","pages":"e10000"},"PeriodicalIF":1.8,"publicationDate":"2025-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143381463","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":"A Novel Method to Determine the Carbon Isotopic Composition of Inositol Hexaphosphate (Phytate) in Soil by Gas Chromatography–Combustion–Isotope Ratio Mass Spectrometry","authors":"V. Sarangi,&nbsp;M. Spohn","doi":"10.1002/rcm.9998","DOIUrl":"https://doi.org/10.1002/rcm.9998","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Understanding the decomposition of inositol hexaphosphate (phytate), the dominant form of organic phosphorus (OP) in soil, is vital for studying phosphorus (P) cycling in terrestrial ecosystems. However, the lack of multiple stable P isotopes complicates the study of phytate dynamics under natural conditions and over long periods.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>A novel method is presented to determine the carbon isotopic composition of inositol in phytate using compound-specific isotope analysis. For this purpose, phytate was extracted from soil and purified via ion exchange chromatography, followed by dephosphorylation, derivatization, and analysis using GC-MS and GC-C-IRMS. Pure compounds were also analyzed to assess protocol efficiency, identify isotopic fractionations, and apply isotopic corrections due to derivatization.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Phytate extracted from soil samples was identified using GC-MS chromatograms. Replicate analyses of the pure compounds indicated that the protocol is highly reproducible. The carbon isotopic composition (δ¹³C) showed a high reproducibility, with values varying by less than 0.5‰ and with no detectable isotopic fractionation during sample preparation. The δ¹³C values of phytate in soil samples reflected the dominant vegetation type (C₃ or C₄) growing at the study site.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>This study offers a novel approach of determining δ¹³C values of inositol of phytate in environmental samples, offering new opportunities to investigate and quantify OP dynamics based on stable carbon isotopes.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.9998","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143380085","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 Laser Ablation ICP-MS Protocol for High-Resolution Iodine-to-Calcium Ratio (I/Ca) Analysis on Corals","authors":"Ashley N. Prow-Fleischer,&nbsp;Zunli Lu","doi":"10.1002/rcm.10002","DOIUrl":"https://doi.org/10.1002/rcm.10002","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Corals are continuous, time-resolved archives of ambient seawater geochemistry and can extend climate records beyond direct monitoring. The iodine-to-calcium (I/Ca) ratio may be a proxy for local oxygen depletion in corals, but the current solution-based ICP-MS protocol limits sampling resolution. A protocol was developed for rapid analysis of coral I/Ca using laser ablation ICP-MS.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Two reference materials, a powdered coral (JCp-1) and a synthetic carbonate (MACS-3), were compared for precision in measuring Sr, Mg, I, Ba, and U. Then, the influence of laser parameters (spot size, fluence, repetition rate, and scan speed) on iodine sensitivity from the reference material was evaluated to optimize laser settings for accurate and reproducible I/Ca calibration. Then, I/Ca was measured in line scans along and across the ambulacrum in a <i>Diploria labyrinthiformis</i> coral.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>We find that JCp-1 has greater precision in measuring iodine, as well as other traces, compared to MACS-3. At a 10 Hz repetition rate, spot sizes from 150 to 85 μm obtained concentrations in agreement with certified values, but higher repetition rates overestimated iodine concentrations from JCp-1. Certain scan speeds and fluence can introduce noise, likely due to matrix effects, but the signal-to-noise ratio can be improved by adjacent-average filtering. Using this simple data filtering routine and optimized laser settings, the highest resolution for accurate I/Ca analysis is &lt; 100 μm. While the fine-scale (&lt; 250 μm) I/Ca variabilities in parallel transects in a coral sample likely resulted from biomineralization processes, large -scale features (&gt; 500 μm) along the ambulacrum tend to correlate.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>LA-ICP-MS has great potential for accurate, high-resolution I/Ca profiling in corals using JCp-1 as a calibration standard. Because of compositional variability near centers of calcification, it is important to pay attention to how the laser transect is aligned relative to skeletal elements, which may incorporate iodine differently.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10002","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143370097","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":"Detection of 4-CPA and Its Related Metabolites Based on LC-QE-HF-MS Technology: A Study on the Impact of Doping Test on the Intake Pathways of Chlorphenesin Carbamate and Chlorphenesin","authors":"Wennuo Xu,&nbsp;Jiahui Cheng,&nbsp;Zhongquan Li,&nbsp;Bing Niu,&nbsp;Xiaojun Deng,&nbsp;Bing Liu","doi":"10.1002/rcm.10004","DOIUrl":"https://doi.org/10.1002/rcm.10004","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Objective</h3>\u0000 \u0000 <p>This study focused on meclofenoxate and its metabolite 4-CPA in the field of doping control and examined the urinary metabolism of chlorphenesin carbamate and chlorphenesin, two substances that may produce 4-CPA.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>A liquid chromatography-Q Exactive-HF-Orbitrap-mass spectrometry (LC-QE-HF-MS)–based assay was developed and validated for the accurate detection of the metabolites of 4-CPA, chlorphenesin carbamate, and chlorphenesin and verified by human subject investigations. Human subjects were studied for three different modes of ingestion (chlorphenesin carbamate administration, sunscreen application containing chlorphenesin, and sunscreen spray application), and urine samples were collected before and after the administration to study the excretion profile of metabolites such as 4-CPA.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The developed assay meets the routine testing requirements of the World Anti-Doping Agency. Following oral administration of chlorphenesin carbamate, 4-CPA levels in the urine ranged from 390 to 6929 ng·mL⁻¹, reaching their maximum concentrations in 12–24 h, with two volunteers having values over the reporting limit. The highest excretion happened 12–24 h after the treatment and continued until 168–264 h later. The C_max of 4-CPA was 1354–2063 and 340 ng·mL⁻¹ after application of sunscreen and spray sunscreen spray, respectively. Maximum excretion of other relevant metabolites was also concentrated at 12–24 h post-dose.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusion</h3>\u0000 \u0000 <p>The results suggest that when measuring 4-CPA, the target analyte of meclofenoxate, in sports drug testing, special consideration needs to be given to whether volunteers have ingested normal therapeutic drugs, such as chlorphenesin carbamate, to avoid misreporting of meclofenoxate results. This finding offers crucial decision support for doping control.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362526","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":"Spatial Proteomics by Parallel Accumulation-Serial Fragmentation Supported MALDI MS/MS Imaging: A First Glance Into Multiplexed and Spatial Peptide Identification","authors":"Mujia Jenny Li,&nbsp;Larissa Chiara Meyer,&nbsp;Nadine Meier,&nbsp;Jannik Witte,&nbsp;Maximilian Maldacker,&nbsp;Adrianna Seredynska,&nbsp;Julia Schueler,&nbsp;Oliver Schilling,&nbsp;Melanie Christine Föll","doi":"10.1002/rcm.10006","DOIUrl":"https://doi.org/10.1002/rcm.10006","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>In spatial proteomics, matrix-assisted laser desorption/ionization (MALDI) imaging enables rapid and cost-effective peptide measurements. Yet, in situ peptide identification remains challenging. Therefore, this study aims to integrate the trapped ion mobility spectrometry (TIMS)–based parallel accumulation-serial fragmentation (PASEF) into MALDI imaging of tryptic peptides to enable multiplexed MS/MS imaging.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>An initial MALDI TIMS MS1 survey measurement was performed, followed by a manual generation of a precursor list containing mass over charge values and ion mobility windows. Inside the dual TIMS system, submitted precursors were trapped, separately eluted by their ion mobility and analyzed in a quadrupole time-of-flight device, thereby enabling multiplexed MALDI MS/MS imaging. Finally, precursors were identified by peptide to spectrum matching.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>This study presents the first multiplexed MALDI TIMS MS/MS imaging (iprm-PASEF) of tryptic peptides. Its applicability was showcased on two histomorphologically distinct tissue specimens in a four-plex and five-plex setup. Precursors were successfully identified by the search engine MASCOT in one single MALDI imaging experiment for each respective tissue. Peptide identifications were corroborated by liquid–chromatography tandem mass spectrometry experiments and fragment colocalization analyses.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>In this study, we present a novel pipeline, based on iprm-PASEF, that allows the multiplexed and spatial identification of tryptic peptides in MALDI imaging. Hence, it marks a first step towards the integration of MALDI imaging into the emerging field of spatial proteomics.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"39 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.10006","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143248379","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}