Journal of Mass Spectrometry最新文献

{"title":"The Impact of Different Alkylation Quenching Methods on Tryptic Activity and Protein Identification in Proteomics Sample Preparation","authors":"Yuan Gao,&nbsp;Min Wang,&nbsp;Lulu Wang,&nbsp;Xinglong Jia,&nbsp;Chunqiu Hu,&nbsp;Ping Liu,&nbsp;Bin Liu,&nbsp;Minjia Tan,&nbsp;Linhui Zhai","doi":"10.1002/jms.5141","DOIUrl":"https://doi.org/10.1002/jms.5141","url":null,"abstract":"<div>\u0000 \u0000 <p>The reduction and alkylation steps are crucial in shotgun proteomics sample preparation to ensure efficient protein digestion and prevent the reformation of artefactual disulfide bonds following proteolysis. Excessive alkylation reagents can lead to overalkylation side reactions, compromising the quality of proteomics sample detection. Previous research has predominantly focused on comparing the effects of various types or concentrations of reducing agents or alkylating reagents for proteomic sample preparation. However, there is a lack of studies systematically comparing the utilization of quenching agents for alkylation reactions and investigating their specific impact on tryptic digestion activity in proteomics sample preparation under conditions of excessive alkylation reagents. In this study, we comprehensively compared the impacts of three different alkylation quenching methods (including cysteine quenching, dithiothreitol [DTT] quenching, and no quenching) on proteomic sample preparation. The upstream sample processing included reduction with DTT or tris(2-carboxyethyl)phosphine (TCEP), followed by alkylation with iodoacetamide (IAA) or chloroacetamide (CAA). Our study demonstrates that the choice of quenching method significantly affects the number of identified proteins and peptides, missed cleavage rates at lysine or arginine residues during trypsin digestion, and the occurrence of overalkylation side reactions. Importantly, our findings indicate that cysteine quenching effectively preserves trypsin activity, ensuring high-quality protein sample preparation. This study provides a systematic analysis of various alkylation quenching methods in proteomic sample preparation and offers optimized experimental protocols and valuable data references for proteomics studies.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 6","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143925774","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 of a Rapid LC-MS/MS Method and Its Application for the Pharmacokinetic Analysis of Pacritinib in Rats","authors":"Ya Meng Wu,&nbsp;Kai Zheng,&nbsp;Luo Yi Huang,&nbsp;Jing Huan Ni,&nbsp;Peng Fei Tang,&nbsp;Jian Chang Qian,&nbsp;Zhong Xiang Xiao,&nbsp;Yun Lei Li","doi":"10.1002/jms.5142","DOIUrl":"https://doi.org/10.1002/jms.5142","url":null,"abstract":"<p>Pacritinib is a novel medication with certain limitations and unknowns in therapeutic applications. Due to the increased frequency of side effects such as fungal infections, nausea, and vomiting, the potential for drug interactions is significantly heightened. This study aimed to establish a quantitative analysis method for pacritinib and investigate its interactions with other drugs. A quantitative detection method for pacritinib in rat plasma was developed using LC-MS/MS, with ibrutinib as an internal standard. This method was subsequently applied to pharmacokinetic and drug–drug interaction studies in rats. The method demonstrated good linearity within the range of 1–1500 ng/mL, with an LLOQ of 1 ng/mL. Both intraday and interday precisions (RSD%) were less than 14.52%, and the recovery, matrix effect, and stability met FDA guidelines. The method proved effective for the quantitative detection of pacritinib in rat plasma. Pharmacokinetic studies revealed that isavuconazole significantly inhibited the metabolism of pacritinib compared to voriconazole, resulting in a 2.5-fold increase in <i>AUC</i>_{(0−<i>t</i>)}, a 2.6-fold increase in <i>AUC</i>_(0–∞), and a 3.0-fold increase in <i>C</i>_<i>max</i>. Additionally, the <i>CLz</i>/<i>F</i> value in the isavuconazole group decreased by 67%. This study successfully established a reliable LC-MS/MS method for detecting pacritinib plasma concentrations in rats. The findings indicate that isavuconazole is more likely to increase pacritinib blood exposure than voriconazole, highlighting the need for caution when combining isavuconazole with pacritinib in clinical practice.</p>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jms.5142","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143889038","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":"Ultra-High Performance Liquid Chromatography–Tandem Mass Spectrometry Method Development and Validation to Quantify Simultaneously Six Urinary DIALKYL Phosphate Metabolites of Organophosphorus Pesticides","authors":"Ngo Kien Đuc,&nbsp;Truong Nhat Khanh,&nbsp;Phan Nguyen Truong Thang,&nbsp;Tran Viet Hung,&nbsp;Pham Diem Thu,&nbsp;Le Thi Bich Chi,&nbsp;Vo Thi Kim Khuyen,&nbsp;Nguyen Duc Tuan","doi":"10.1002/jms.5128","DOIUrl":"https://doi.org/10.1002/jms.5128","url":null,"abstract":"<div>\u0000 \u0000 <p>The exposure to chemical pesticides is one of the world's concerns, especially in Vietnam, which is becoming a key player in global agriculture. The chronic long-term exposure to pesticides, especially organophosphorus groups poses increased health risks such as cancer and related diseases due to their hazardous metabolites. The characterization of urinary pesticides is essential to understand the pesticide exposure patterns. Therefore, this research aims to develop a liquid chromatography–tandem mass spectrometry procedure for the quantification of six dialkyl phosphate metabolites of organophosphorus pesticides based on simulated human urine containing dialkyl phosphates and urine samples of organophosphorus pesticides-exposed farmers in An Giang province of Vietnam. As a result, a highly sensitive procedure with a negative ion atmospheric pressure chemical ionization source, fosfomycin as internal standard and multireaction monitoring, was successfully validated in compliance with international guidelines for simultaneous quantitative determination of six dialkyl phosphates in human urine samples. Molecular and fragmented ions for quantification were consistent with the standard spectrum. The linear ranges of DMP, DEP, DMTP, DETP, DMDTP, and DEDTP were 5.29–1000.58, 5.10–1000.19, 5.10–1000.20, 5.06–1000.11, 5.06–1000.11, 5.30–1000.60, and 5.06–1000.12 ng/mL, respectively. The validation results showed that the selectivity, intraday and interday precision and accuracy, matrix effect, carry over, dilution, and stability of all the analytes were in the acceptable range. In total, 383 spot urine samples from people working with pesticides were satisfactorily analyzed by the proposed procedure. Over 80% of farmers were detected with at least one organophosphate metabolite, especially DEDTP with high concentrations, up to 5015.0 ng/mL, which alerts the high likelihood of pesticide exposure in the community of rural areas in Vietnam.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143879932","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 Identification of Chemical Compounds in Danzhi Jiangtang Capsule Using Ultra-Performance Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry Combined With Multiple Data Processing Techniques","authors":"Xiaojie Fu,&nbsp;Junting Zhou,&nbsp;Jindong Zhao,&nbsp;Rui Yang,&nbsp;An Zhou,&nbsp;Zhaohui Fang,&nbsp;Huan Wu","doi":"10.1002/jms.5140","DOIUrl":"https://doi.org/10.1002/jms.5140","url":null,"abstract":"<div>\u0000 \u0000 <p>Danzhi Jiangtang capsule (DJC) is a traditional Chinese medicine prescription that has been clinically used to treat Type 2 diabetes mellitus and its complications. However, research on the chemical compounds present in DJC remains limited. In this study, an analytical strategy based on ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) was developed for the rapid and systematic characterization of chemical compounds in DJC. Firstly, a DJC self-built database was established, and UPLC-Q-TOF/MS was applied for comprehensive profiling of DJC's chemical compounds. Then, <i>R</i> language combined with MZmine was used for data preprocessing to construct the ion information list and extract effective data. Finally, the compounds were identified by multiple data processing techniques (multiple-point screening mass defect filtering [MDF], extracted ion chromatogram [EIC], neutral loss filter [NLF], diagnostic fragment ion filtering [DFIF], and direct identification method [including retention time, fragment behavior and reference substances]). Eventually, 137 compounds were characterized from DJC, including 19 monoterpenoids, 26 triterpenoids, 8 flavonoids, 12 iridoids, 7 phenylethanoid glycosides, 8 acetophenones, 23 organic acids, 2 violet ketones, 13 cyclic peptides, 8 alkaloids, 2 fatty acids, and 9 other compounds. Among these, 16 compounds were verified using reference substances. The study indicated that the analytical strategy established in this study effectively supports the in-depth study of DJC's chemical constituents and provides essential data for subsequent in vivo studies.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143875528","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":"Identification of Botanicals Based on Their Mass Spectrum Fingerprints Using Ultra-Performance Liquid Chromatography-Mass Spectrometry","authors":"Akhilesh Kumar,&nbsp;Dipak Kumar Mishra,&nbsp;Sanjeev Kanojiya","doi":"10.1002/jms.5131","DOIUrl":"https://doi.org/10.1002/jms.5131","url":null,"abstract":"<div>\u0000 \u0000 <p>In the current scenario, herbal raw materials are identified via morphotaxonomy, microscopic pharmacognosy, or DNA barcoding. However, these methods do not reveal their chemical integrity, while plant raw materials play a crucial role in the quality of plant-based medicine. To overcome this limitation, we used a mass spectrometry-based method to identify 30 botanicals. This assay followed a standard operating procedure (SOP) from sample preparation to the reference library's mass spectrum fingerprint (MSFP) search. The MS1 score showed a similarity index between the input data and the reference mass spectrum. A more than 50% MS1 score was the critical threshold for accurately identifying botanicals based on their chemical integrity. Interestingly, the analysis of 30 different plant species yielded no false results. The results were 100% accurate and selective for tested botanical samples. However, we found that the standard deviation of analytical assays and biological replicates was ± 3.5 and ± 6.3 (MS1 score) for all analyzed samples, respectively. Intraspecies variability showed MS1 scores &gt; 50% ± 10, whereas interspecies variability was observed with MS1 scores &lt; 50% ± 10. The MS1 score was observed, dependent on the plant species, ranging from 53.00% (± 2.65) to 89.76% (± 4.08). In addition, the method was tested to see how seasonal and geographical changes affected search results. The MS1 score changed by less than 15%. We simultaneously created a chemical barcode (unique molecular weight sequence) for each plant species to validate search results and ensure the reliable identification of botanicals.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143856959","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":"Spatially Resolved Metabolomics Reveals Metabolic Heterogeneity Among Pulmonary Fibrosis","authors":"Shengxi Li,&nbsp;Cong Li,&nbsp;Wei Sun,&nbsp;Yinghao Cao,&nbsp;Xianmei Qi,&nbsp;Jiawei Zhang,&nbsp;Yanjiang Xing,&nbsp;Jinyu Zhou,&nbsp;Lin Wang","doi":"10.1002/jms.5138","DOIUrl":"https://doi.org/10.1002/jms.5138","url":null,"abstract":"<div>\u0000 \u0000 <p>Pulmonary fibrosis (PF) is a chronic and progressive lung disease with fatal consequences. The study of PF is challenging due to the complex mechanism involved, the need to understand the heterogeneity and spatial organization within lung tissues. In this study, we investigate the metabolic heterogeneity between two forms of lung fibrosis: idiopathic pulmonary fibrosis (IPF) and silicosis, using advanced spatially-resolved metabolomics techniques. Employing high-resolution mass spectrometry imaging, we spatially mapped and identified over 260 metabolites in lung tissue sections from mouse models of IPF and silicosis. Histological analysis confirmed fibrosis in both models, with distinct pathological features: alveolar destruction and collagen deposition in IPF, and nodule formation in silicosis. Metabolomic analysis revealed significant differences between IPF and silicosis in key metabolic pathways, including phospholipid metabolism, purine/pyrimidine metabolism, and the TCA cycle. Notably, phosphocholine was elevated in silicosis but reduced in IPF, while carnitine levels decreased in both conditions. Additionally, glycolytic activity was increased in both models, but TCA cycle intermediates showed opposing trends. These findings highlight the spatial metabolic heterogeneity of PF and suggest potential metabolic targets for therapeutic intervention. Further investigation into the regulatory mechanisms behind these metabolic shifts may open new avenues for fibrosis treatment.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861540","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":"Sulfuric/Sulfurous Acids Induce Self-Protection of Phospholipids Against Air–Water Interfacial Ozonolysis","authors":"Hong Zhang,&nbsp;Yuqing Niu,&nbsp;Jiaqi Xing,&nbsp;Jing He,&nbsp;Yuexin Zhang,&nbsp;Lina Qiao,&nbsp;Panpan Bai,&nbsp;Xiangnan Zhang,&nbsp;Jie Jiang","doi":"10.1002/jms.5139","DOIUrl":"https://doi.org/10.1002/jms.5139","url":null,"abstract":"<div>\u0000 \u0000 <p>Sulfides are ubiquity in atmosphere and can convert to be H₂SO₃/H₂SO₄, which could affect the inflammatory responses induced by ozone. However, the mixing effect and mechanism of H₂SO₃/H₂SO₄ and ozone at molecular-level on the lung surface is still indefinable. Herein, using 1-palmitoyl-2-oleoyl-<i>sn</i>-glycero-3-phosphatidylglycerol (POPG) monolayer as a model, effects of H₂SO₄/H₂SO₃ on interfacial ozonolysis of phospholipids were explored. Both H₂SO₄ and H₂SO₃ could decrease ozonolysis efficiencies of POPG and showed a remarkable concentration dependence. The main components of H₂SO₄ and H₂SO₃ in investigated system and their effects on POPG ozonolysis were separately explored, and the mechanism was proposed. The observed decrease of ozonolysis efficiencies resulted from POPG hydrolysis induced by H⁺ and reactive activity of HSO₃⁻ and SO₃²⁻ towards ozone. The hydrolysis of POPG could provide oleic acids, which further lowered the ozonolysis efficiency. In addition, the efficiency of POPG ozonolysis in H₂SO₃ case was lower than that in H₂SO₄ case, and the self-sacrificing oxidation of HSO₃⁻ and SO₃²⁻ by ozone was responsible for this process. Considering extra phospholipids in epithelial lining fluid of lung, the short-term or low concentration exposure of H₂SO₄/H₂SO₃ was thought to trigger the self-protection of lung. However, the long-term or high concentration exposure would lead to irreversible damage.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143856800","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":"Multi-Omic Evaluation of PLK1 Inhibitor—Onvansertib—In Colorectal Cancer Spheroids","authors":"Brian D. Fries,&nbsp;Emily R. Sekera,&nbsp;Joseph H. Holbrook,&nbsp;Amanda B. Hummon","doi":"10.1002/jms.5137","DOIUrl":"https://doi.org/10.1002/jms.5137","url":null,"abstract":"<p>Polo-like kinase 1 (Plk1) is a serine/threonine kinase involved in regulating the cell cycle. It is activated by aurora kinase B along with the cofactors Borealin, INCE, and survivin. Plk1 is involved in the development of resistances to chemotherapeutics such as doxorubicin, Taxol, and gemcitabine. It has been shown that patients with higher levels of Plk1 have lower survival rates. Onvansertib is a competitive ATP inhibitor for Plk1 in clinical trials for the treatment of tumors and has recently entered a trial for the treatment of <i>KRAS</i> mutant colorectal cancers (CRCs). In this study, we conducted an untargeted liquid chromatography–mass spectrometry (LC–MS) proteomics study as well as an untargeted lipidomics analysis of HCT 116 spheroids treated with onvansertib over a 72-h treatment time-course experiment. Mass spectrometry imaging (MSI) showed that onvansertib begins to accumulate most prominently after 12 h of treatment and continues to accumulate through 72 h. Proteomic results displayed alterations to cell cycle control proteins and an increasing abundance of aurora kinase B and Borealin. The proteomics data also showed alterations to many lipid metabolism enzymes. The MSI lipidomics data indicated alterations to phosphatidylcholine lipids, with many lipids increasing in abundance over time or increasing until 12 h of onvansertib treatment and decreasing after that time point. In summary, these results suggest that onvansertib is causing cells within the spheroid to halt at a certain phase of the cell cycle in accordance with previous literature. Our findings suggest the S phase is likely interrupted, with observed alterations in cell cycle control proteins and PC lipid abundance.</p>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jms.5137","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143793527","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":"Collision Cross Section Measurements in Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR MS) Based on the Flipping-Filtering Method","authors":"Dayu Li,&nbsp;Zhiwei Wang,&nbsp;Yanying Fan,&nbsp;Wei Xu","doi":"10.1002/jms.5136","DOIUrl":"https://doi.org/10.1002/jms.5136","url":null,"abstract":"<div>\u0000 \u0000 <p>The ion collision cross section (CCS) is closely related to the structural and physical conformation of compounds, making it an ideal parameter for constructing databases. In recent years, Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) has gained widespread application in CCS measurements thanks to its ultra-high mass resolution and accuracy. Due to the collisions between ions and neutral molecules within the FT-ICR MS cell, the image current decays. Based on this feature, the ion CCS can be precisely calculated by applying corresponding collision models and algorithms. A new time-frequency analysis method is introduced: the flipping-filtering method based on the Levenberg–Marquardt algorithm. Before filtering, the data undergoes flipping and extension, effectively mitigating the issue of signal point waste commonly associated with traditional filtering techniques. This approach ensures a smooth and uninterrupted envelope of the image current signal while significantly enhancing the accuracy of decay factor and ion CCS measurements. Compared to the linewidth correction method and the line shape fitting method, this method exhibits superior noise resistance and resolution capabilities, serving as a valuable adjunct to ion CCS measurement techniques.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143793452","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":"Comparison of Dip-it-DART-Orbitrap-MS With Nitrogen Plasma to HPLC/Orbitrap-MS in Profiling Aromatic Glycoconjugation in White Grapes","authors":"Mariusz Dziadas,&nbsp;Henryk Jeleń","doi":"10.1002/jms.5130","DOIUrl":"https://doi.org/10.1002/jms.5130","url":null,"abstract":"<div>\u0000 \u0000 <p>Direct analysis of aromatic glycosidic precursors in plants has posed an analytical challenge for decades. Traditional techniques, such as SPE-GC/MS, primarily provided information on volatile aglycones released through hydrolysis. However, the application of high-resolution mass spectrometry combined with liquid chromatography has enabled the direct analysis of intact glycosides without the need for derivatization or hydrolysis. Advances in soft ionization methods, such as DART, offer a novel approach to exploring the hidden aromatic potential in grapes without chromatographic separation. In this work, we present a novel and rapid method for screening aromatic glycosidic precursors in white grapes using high-resolution mass spectrometry (Orbitrap) combined with the soft ionization DART method with nitrogen plasma. Optimization of N₂-DART ionization parameters, including grid voltage, gas temperature, and Dip-it sampler speed, performed on selected synthetic glycosidic precursors, allowed the establishment of characteristic ionization patterns and evaluation of 15 groups of glycosidic precursors. The results from the profiling analysis using the N₂-DART-Orbitrap-MS method are comparable to those obtained by HPLC/Orbitrap-MS method. This new analytical approach, N₂-DART-Orbitrap-MS, reduces drastically analysis time by eliminating the need for chromatographic separation when screening glycoside precursors, uses a convenient Dip-it tips for sampling. It also allows for deeper exploration of ionization using nitrogen plasma, applied for the first time in the analysis of glycoside precursors, demonstrating the applicability of this method for the rapid characterization and screening of glycosidically bound aroma compounds in plants.</p>\u0000 </div>","PeriodicalId":16178,"journal":{"name":"Journal of Mass Spectrometry","volume":"60 5","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-04-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143793426","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}