Journal of Mass Spectrometry最新文献

{"title":"Development and Validation of a Candidate Reference Measurement Procedure for Plasma Clozapine Quantification Using ID-LC–MS/MS","authors":"Xiaodong Yang,&nbsp;Minmin Tu,&nbsp;Chunlan Tang,&nbsp;Min Shen,&nbsp;Huoyan Ji","doi":"10.1002/jms.5168","DOIUrl":"10.1002/jms.5168","url":null,"abstract":"<div>\u0000 \u0000 <p>We developed a candidate reference measurement procedure (cRMP) based on isotope dilution liquid chromatography–tandem mass spectrometry (ID-LC–MS/MS) for the accurate quantification of clozapine (CLO) in human plasma. After systematic optimization of chromatographic separation conditions for CLO, we evaluated various sample pretreatment methods. The analytical performance of the cRMP was rigorously validated, encompassing specificity, recovery, precision, linearity, limit of quantitation (LoQ), limit of detection (LoD), carryover, stability, and method comparison. Measurement uncertainties were assessed in accordance with GUM, taking CLO purity, balance weighing, calibration curve, measurement imprecision, recovery, and carryover into account. Under optimized conditions, CLO showed effective separation from potential interferents in human plasma. The method exhibited excellent linearity (<i>R</i>² = 0.9988) across a concentration range of 5.65–1693.51 ng/g. The total coefficients of variation (CVs) were 2.04%, 0.97%, and 0.65% at concentrations of 24.53, 98.06, and 987.02 ng/g, respectively. Average recoveries ranged from 97.80% to 99.28%, with a LoQ of 2.73 ng/g and a LoD of 0.91 ng/g. The expanded measurement uncertainties (<i>U</i>) were 1.3 ng/g (<i>k</i> = 2) at 24.53 ng/g, 3.8 ng/g (<i>k</i> = 2) at 98.06 ng/g, and 35.3 ng/g (<i>k</i> = 2) at 987.02 ng/g. The developed cRMP for CLO quantification demonstrates excellent specificity, accuracy, precision, and traceability, meeting all the criteria for cRMPs. This method has the potential to standardize therapeutic drug monitoring (TDM) for CLO, improving clinical outcomes and patient safety.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 9","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144869733","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":"Paper Spray Mass Spectrometry for In Vivo Dermatopharmacokinetic Study of Skin Drugs by Touch Sampling","authors":"Xing Li,&nbsp;Huicai Wen,&nbsp;Mingzhuo Liu,&nbsp;Zi-Cheng Yuan,&nbsp;Bin Hu,&nbsp;Guanghua Guo","doi":"10.1002/jms.5165","DOIUrl":"10.1002/jms.5165","url":null,"abstract":"<div>\u0000 \u0000 <p>Many viscous drugs are used for the treatment of various skin disorders, but they pose a challenging task for dermatopharmacokinetic (DPK) studies by traditional analytical tools because of complicated processes and time-consuming sample pretreatment. In this work, we applied paper spray mass spectrometry (PSMS) for direct sampling and analysis of seven viscous drugs from the human skin surface. The detection precision was found in the range of 2.9%–20.7% (<i>n</i> = 5); limit of detection (LOD) and limit of quantitation (LOQ) were found at 0.01–0.12 μg and 0.15–0.39 μg, respectively. Moreover, acceptable matrix effect (3.9%–16.3%), accuracy (5.5%–16.6%), and recovery (73.6% - 135.2%) were obtained. Quantification of seven drugs on the skin surface was also performed with good dynamic ranges of three orders of magnitude. DPK studies of seven drugs were investigated for a long time up to 12 h, showing the kinetic curves of exponential function with good coefficients (<i>R</i>² &gt; 0.9). Overall, our results show that PSMS is a powerful tool that integrates sampling, extraction, and microanalysis for DPK study.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 9","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144814837","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":"Rapid Detection and Classification of Mango (Mangifera indica L.) Leaves by Paper Spray Ionization Mass Spectrometry","authors":"Yiqiu Wei,&nbsp;Guanyu Lu,&nbsp;Guohuan Zhang,&nbsp;Yiran Wang,&nbsp;Peiqi Luo","doi":"10.1002/jms.5169","DOIUrl":"10.1002/jms.5169","url":null,"abstract":"<div>\u0000 \u0000 <p>Paper spray ionization mass spectrometry (PSI MS) was developed for natural products detection in mango leaves and mango leaves classification. Rapid detection of plant natural products by PSI MS was achieved without complex sample preparation. Many natural products were detected, including medicinally valuable natural products. Principal component analysis (PCA) was applied for the classification of different mango varieties. The PCA result demonstrated clear differentiation between varieties, such as Guifei, Guiqi, and Tainong. This method offers significant advantages for rapid screening of natural products and evaluation of plant utilization value.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 9","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144815150","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":"Real-Time Proton Transfer Reaction Mass Spectrometry for Pesticide Detection: A DFT-Based Feasibility Evaluation","authors":"Yuliang Huang,&nbsp;Tong Yang,&nbsp;Chunguang Xie,&nbsp;Ping Cheng","doi":"10.1002/jms.5163","DOIUrl":"10.1002/jms.5163","url":null,"abstract":"<div>\u0000 \u0000 <p>This feasibility study evaluates the application of proton transfer reaction mass spectrometry (PTR-MS) for the online measurement of pesticides. Although PTR-MS has established its efficacy in detecting volatile organic compounds, its potential for pesticide detection remains underexplored. DFT calculations were performed at the B3LYP/6-311++G(d,p) level to predict essential molecular properties, including dipole moments, polarizabilities, proton affinities, and ionization energies. These calculations provided insights into the thermodynamics of ion–molecule reactions, revealing that most pesticides exhibit favorable ionization reactions with H₃O⁺ and NO⁺, whereas NH₄⁺ may present challenges for certain compounds like fenitrothion. Additionally, we calculated ion–molecule reaction rate constants, which facilitate quantification without prior standard calibration. This study lays the groundwork for the future development of real-time pesticide residue monitoring techniques based on PTR-MS, with potential application in food safety and environmental monitoring.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 9","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144814835","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":"Analysis of Saposhnikoviae Radix and Libonotidis Radix Based on “Characteristic Ion Set” and Chemometrics","authors":"Xianrui Wang,&nbsp;Fangliang He,&nbsp;Haonan Wu,&nbsp;Wenguang Jing,&nbsp;Minghua Li,&nbsp;Xiaohan Guo,&nbsp;Xianlong Cheng,&nbsp;Feng Wei","doi":"10.1002/jms.5164","DOIUrl":"10.1002/jms.5164","url":null,"abstract":"<p>To enrich detection methods of Saposhnikoviae Radix (SR) adulterated Libonotidis Radix (LR) and improve the screening efficiency, this paper conducted an analysis of SR and LR based on chemometrics and “characteristic ion set.” Firstly, the samples were analyzed by liquid chromatography-mass spectrometer and converted into data matrix. After feature algorithm extraction, the “characteristic ion set” of SR and LR was obtained to match the test and blind market samples for feedback matching index (MI). In addition, the LR proprietary component was extracted to verify the MI analysis based on “characteristic ion set.” Three percent LR adulteration was identified based on “characteristic ion set,” and two market blind samples were identified as adulterated samples. Xanthalin was the LR proprietary component. Moreover, the analysis based on “characteristic ion set” is reliable through chemometric analysis and extraction of proprietary ions. “Characteristic ion set” and chemometrics can enrich the detection methods of SR and LR and improve the screening efficiency.</p>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 9","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/epdf/10.1002/jms.5164","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144814836","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":"Comprehensive Strategy Analysis of Chemical Constituents of Xiaoliu Powder Based on GC–MS and UPLC-Q-Exactive Orbitrap MS","authors":"Jinyuan Bai,&nbsp;Yatong Wang,&nbsp;Na Zhang,&nbsp;Jianhai Wang,&nbsp;Boyang Shang,&nbsp;Guodong Qin,&nbsp;Min Zhao","doi":"10.1002/jms.5160","DOIUrl":"10.1002/jms.5160","url":null,"abstract":"<div>\u0000 \u0000 <p>Few studies on Xiaoliu Powder (XLP) have been reported; it is necessary to clarify the material basis of XLP to lay a foundation for further clarifying its mechanism of action and supporting rational drug use. This study aims to comprehensively analyze the chemical constituents of XLP by GC–MS and UPLC-Q-Exactive Orbitrap MS, with the aim of identifying its volatile and nonvolatile components and providing insights into its pharmacological properties. Volatile components were extracted and analyzed by GC–MS, and 37 compounds were detected, accounting for 72.58% of the total peak area. Aldehydes were found to be the predominant group, followed by alkenes, esters, and phenolic compounds. Nonvolatile components were identified through UPLC-Q-Exactive Orbitrap MS, leading to the detection of 126 compounds, including triterpenoids, flavonoids, phenylpropanoids, organic acids, and other classes of compounds. A total of 13 compounds were accurately identified by comparison with reference standards. The findings suggest that XLP contains a diverse range of bioactive compounds, which may contribute to its therapeutic effects. A comprehensive chemical profile of XLP has been established, providing a solid foundation for further research on its pharmacological mechanisms and clinical applications.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 9","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144815148","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 Mapping of Gangliosides and Proteins in Amyloid Beta Plaques at Cellular Resolution Using Mass Spectrometry Imaging and MALDI-IHC","authors":"Christopher J. Good,&nbsp;Andrew P. Bowman,&nbsp;Corinna Klein,&nbsp;Khader Awwad,&nbsp;Wayne R. Buck,&nbsp;Junhai Yang,&nbsp;David S. Wagner","doi":"10.1002/jms.5161","DOIUrl":"10.1002/jms.5161","url":null,"abstract":"<p>In pharmaceutical research and development, technologies like mass spectrometry imaging (MSI) offer spatially resolved compound distributions to aid in the discovery of drug targets and development of drug candidates. Through traditional and immunohistochemical approaches centered around MSI, distributions of endogenous lipids and proteins can be mapped on the same tissue section at cellular resolution. To highlight the cellular resolution capability of the integrated MSI workflow leveraged here, an animal model of Alzheimer's disease (<span>AD</span>) was interrogated due to the relationship of lipid dysregulation and extracellular protein deposition in driving disease pathology, especially at the site of amyloid beta (Aβ) plaques. Gangliosides, Aβ peptides, and microglia were imaged at 5 μm spatial resolution in the brains of an APPPS1 mouse model. GM3 and GM2 gangliosides displayed plaque-associated accumulation as supported by previous studies of a range of AD models. Advanced methods for achieving cellular resolution imaging of lipids and proteins have revealed heterogeneity in molecular distributions, which appears to be influenced by the microenvironment surrounding Aβ plaques. While these data could support future biological conclusions of AD, a central aim of this study was to emphasize the potential impact of an MSI workflow, which fuses spatial lipidomic and proteomic data at cellular resolution, on translational drug discovery research. This dual molecular imaging approach and data mining strategy can not only support efforts in the discovery of novel drug targets, but also in evaluating drug-target engagement when the distribution of a small molecule drug is simultaneously investigated.</p>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 9","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/epdf/10.1002/jms.5161","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144815149","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":"Transfer-Based Thin-Section-Free MALDI Mass Spectrometry Imaging Using a Platinum-Coated Porous Plate Formed of Glass Beads","authors":"Takamasa Ikeda","doi":"10.1002/jms.5162","DOIUrl":"10.1002/jms.5162","url":null,"abstract":"<div>\u0000 \u0000 <p>Matrix- and surface-assisted laser desorption/ionization mass spectrometry imaging (MALDI- and SALDI-MSI) are widely used for visualizing molecular distributions not only in medical and pharmaceutical applications but also in plant and food analysis. To overcome limitations associated with sample hardness or fragility, a transfer-based approach was recently developed as an alternative to thin sectioning. In particular, Pt-coated porous plates formed of glass beads (transfer plates) have been introduced as robust substrates for thin-section-free SALDI-MSI. In this study, we demonstrate for the first time that these transfer plates also support thin-section-free MALDI-MSI by transferring the entire strawberry cross-section onto the plate. First, SALDI-MSI was performed; then, a matrix was applied to the same sample on the transfer plate, which was followed by MALDI-MSI. Sequential imaging using both modalities enabled comparison under identical conditions. Ion images of hexose, citric acid, and sucrose obtained using both modalities showed qualitative agreement, indicating that the prior SALDI-MSI and the delocalization caused by subsequent matrix spraying had no substantial effect on the MALDI-MSI results while using a 200-μm step size. In addition, anthocyanins localized to the strawberry skin, which could not be detected by SALDI-MSI, were successfully visualized by MALDI-MSI, thereby validating the method. These results confirm that MALDI-MSI can be performed on transfer plates without sectioning, expanding the utility of this sampling platform. The proposed approach utilizing a transfer plate enables efficient acquisition of both SALDI and MALDI data, which is particularly useful when conventional sectioning or sample duplication is impractical.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 9","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144815176","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":"Development and Validation of an UPLC-MS/MS Method for Simultaneous Quantification of Bisoprolol and Hydrochlorothiazide in Human Plasma","authors":"Asmaa Al-Asmar,&nbsp;Naim Kittana,&nbsp;Abdallatif Mayyala,&nbsp;Ibrahim Asmar,&nbsp;Amjad Hussein","doi":"10.1002/jms.5159","DOIUrl":"10.1002/jms.5159","url":null,"abstract":"<div>\u0000 \u0000 <p>Bioanalytical method development and validation are essential for reliable quantification of drugs in biological matrices. This research focuses on developing and validating a UPLC-MS/MS method for the simultaneous determination of bisoprolol and hydrochlorothiazide in human plasma, adhering to established regulatory guidelines for bioanalytical method validation. The development and validation focus on creating a robust and sensitive assay suitable for bioequivalence studies and routine therapeutic drug monitoring. This method utilizes bisoprolol D5 and hydrochlorothiazide C13 D2 as internal standards to enhance accuracy and precision. Chromatographic separation was achieved on a Waters Acquity UPLC BEH C18 column (100 × 2.1 mm, 1.7 μm particle size) with an isocratic mobile phase consisting of 10 mM ammonium formate buffer, methanol, and 0.1% ammonia solution (10:90, v/v). The flow rate was set at 0.3 mL/min, with a retention time of 2.2 min. Multiple reaction monitoring (MRM) was used with positive ESI for bisoprolol (m/z 326.36 → 116.13, internal standard m/z 331.36 → 121.13) and negative ESI for hydrochlorothiazide (m/z 296.11 → 269.00, internal standard m/z 299.11 → 270.00). The analytes and their respective internal standards were co-extracted using a liquid–liquid extraction method with <i>tert</i>-butyl methyl ether as the extraction solvent. Linearity for bisoprolol and hydrochlorothiazide was maintained over a concentration range of 1–100 ng/mL for bisoprolol and 1.0–300 ng/mL for hydrochlorothiazide, respectively, using a weighted least squares linear regression model (1/x). This method achieved a lower limit of quantification (LLOQ) of 1.0 ng/mL, making it highly sensitive for the detection of these analytes. Moreover, the method demonstrated high accuracy, precision, selectivity, and reduced overall analysis time, making it well suited for routine analysis and bioequivalence studies of 10 mg bisoprolol and 25 mg hydrochlorothiazide tablets.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 8","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-07-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144714736","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":"Improved Annotation of Internal Fragments via Trapped-Ion Mobility Enhanced Top-Down Sequencing of Protein Ions","authors":"Katherine A. Graham,&nbsp;Charles F. Lawlor,&nbsp;Rachitha S. Reddy,&nbsp;Supadach Prertprawnon,&nbsp;Olakunle O. Akinola,&nbsp;Vincent J. Grisolia,&nbsp;Keshari Kunwor,&nbsp;Nicholas B. Borotto","doi":"10.1002/jms.5158","DOIUrl":"10.1002/jms.5158","url":null,"abstract":"<p>Analysis of intact protein ions allows for valuable insights into complex biological processes. However, top-down mass spectrometry data is often convoluted and frequently results in numerous overlapping product ions. Ion mobility spectrometry (IMS) can aid in the deconvolution of these spectra, and we previously demonstrated that the IMS separations provided by trapped IMS (TIMS) significantly increased the sequence coverage provided by collision induced dissociation (CID). In this work, we further improve the “CIDtims” method by incorporating the dynamic control of ion populations, optimizing the bioinformatic approach to better leverage the mobility separation, and finally porting the technique to an improved version of the instrument, the timsTOF Pro2. Lastly, we utilize these improvements to assess internal ions generated by CIDtims. Internal ions are of particular importance in the CIDtims workflow as all charge states are simultaneously activated and the highest charge states will likely be subjected to “over fragmentation.” We demonstrate that mobility separation increases the signal-to-noise ratios and the isotopic fit scores of internal ions and enables the assignment of additional product ions.</p>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 8","pages":""},"PeriodicalIF":2.0,"publicationDate":"2025-07-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jms.5158","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144647036","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}