European Journal of Mass Spectrometry最新文献

{"title":"Hammett correlation in competition experiments in dissociation of ionised substituted benzophenones and dibenzylideneacetones.","authors":"Nathan W Fenwick,&nbsp;Richard Telford,&nbsp;William H C Martin,&nbsp;Richard D Bowen","doi":"10.1177/14690667231184363","DOIUrl":"https://doi.org/10.1177/14690667231184363","url":null,"abstract":"<p><p>A convenient method of applying competition experiments to devise a Hammett correlation in the dissociation by α-cleavage of 17 ionised 3- and 4-substituted benzophenones, YC₆H₄COC₆H₅ [Y=F, Cl, Br, CH₃, CH₃O, NH₂, CF₃, OH, NO₂, CN and N(CH₃)₂] is reported and discussed. The results given by this approach, which rely on the relative abundance of [M-C₆H₅]⁺ and [M-C₆H₄Y]⁺ ions in the electron ionisation spectra of the substituted benzophenones, are compared with those obtained by previous methods. Various refinements of the method are considered, including reducing the ionising electron energy, making allowance for the relative abundance of ions such as C₆H₅⁺ and C₆H₄Y⁺, which may be formed to some extent by secondary fragmentation, and using substituent constants other than the standard σ constants. The reaction constant, ρ, of 1.08, which is in good agreement with that deduced previously, is consistent with a considerable reduction in electron density (corresponding to an increase in positive charge) at the carbon of the carbonyl group during fragmentation. This method has been successfully extended to the corresponding cleavage of 12 ionised substituted dibenzylideneacetones, YC₆H₄CH=CHCOCH=CHC₆H₅ (Y=F, Cl, CH₃, OCH₃, CF₃, and NO₂), which may fragment to form either a substituted cinnamoyl cation, [YC₆H₄CH=CHCO]⁺, or the cinnamoyl cation, [C₆H₅CH=CHCO]⁺. The derived ρ value of 0.76 indicates that the substituent, Y, influences the stability of the cinnamoyl cation somewhat less strongly than it does the analogous benzoyl cation.</p>","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 4","pages":"211-219"},"PeriodicalIF":1.3,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10466955/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10126170","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Identification and characterization of stress degradation products of ibrutinib by LC-UV/PDA and LC-Q/TOF-MS studies.","authors":"Bidisha Mondal,&nbsp;Alka Bali,&nbsp;Tanvi Sharma","doi":"10.1177/14690667231194814","DOIUrl":"https://doi.org/10.1177/14690667231194814","url":null,"abstract":"<p><p>The anticancer drug ibrutinib was subjected to stress degradation studies under the ICH-prescribed hydrolytic, photolytic, oxidative and thermal stress conditions, and its degradation behavior was studied. A significant degradation was noted for the drug under acidic/alkaline hydrolytic, acid/alkaline photolytic, and oxidative conditions. The UPLC-UV/PDA studies revealed the generation of six degradation products (<b>I-VI</b>), and these were adequately resolved from the drug under the developed chromatographic conditions over a Kinetex® C18 (100 mm×4.6 mm; 2.6 μm) column employing isocratic elution method. Detection wavelength was selected as 289 nm. The UPLC-UV/PDA method conditions were extrapolated to UPLC-MS/TOF studies. All the six degradation products were found to be ionized in the total ion chromatogram, and the products could be identified and characterized from their mass spectral data. The possible degradation route of ibrutinib leading to generation of various products was also postulated.</p>","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 4","pages":"248-261"},"PeriodicalIF":1.3,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10421218","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Protonation of gabapentin: Ion mobility spectrometry and computational study.","authors":"Manijeh Tozihi,&nbsp;Hamed Bahrami,&nbsp;Mohammadreza Zarifian,&nbsp;Morteza Vahedpour","doi":"10.1177/14690667231184106","DOIUrl":"https://doi.org/10.1177/14690667231184106","url":null,"abstract":"<p><p>Protonation of gabapentin was studied using corona discharge ion mobility spectrometry with two types of reactant ions at temperature of 200°C. It was found that at elevated temperatures, ionization of gabapentin proceeds via two channels, including the protonation and reactant ion attachment, in the presence of both hydronium and ammonium reactant ions. The effect of the sample concentration on the relative intensity of product ion peaks was also studied. It turned out that in high concentrations, in addition to the protonation of gabapentin, binding of the reactant ion and the formation of proton-bound dimer also occurred, while in low concentrations, the only product of the ionization process is protonated gabapentin. Density functional theory (DFT) with B3LYP and M062X functionals employing the same basis set 6-311++G(d,p) was used to extend the experimental findings. The structures of the several conformers of neutral and protonated gabapentin were obtained. Based on them, topical proton affinity and topical gas-phase basicity of gabapentin were calculated for selected conformers. The attachment of reactant ions to neutral gabapentin and formation of proton-bound dimer were thermodynamically studied.</p>","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 4","pages":"220-230"},"PeriodicalIF":1.3,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10055169","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Corrigendum.","authors":"","doi":"10.1177/14690667231195424","DOIUrl":"https://doi.org/10.1177/14690667231195424","url":null,"abstract":"","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 4","pages":"272"},"PeriodicalIF":1.3,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10432291","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Long-term <i>in situ</i> air quality assessment in closed environments: A gas chromatography-ion mobility spectrometry applicability study.","authors":"Pedro Catalão Moura,&nbsp;Valentina Vassilenko","doi":"10.1177/14690667231187502","DOIUrl":"https://doi.org/10.1177/14690667231187502","url":null,"abstract":"<p><p>Contemporary life is mostly spent in indoor spaces like private houses, workplaces, vehicles and public facilities. Nonetheless, the air quality in these closed environments is often poor which leads to people being exposed to a vast range of toxic and hazardous compounds. Volatile organic compounds (VOCs) are among the main factors responsible for the lack of air quality in closed spaces and, in addition, some of them are particularly hazardous to the human organism. Considering this fact, we conducted daily <i>in situ</i> air analyses over 1 year using a gas chromatography-ion mobility spectrometry (GC-IMS) device in an indoor location. The obtained results show that 10 VOCs were consistently present in the indoor air throughout the entire year, making them particularly important for controlling air quality. All of these compounds were successfully identified, namely acetic acid, acetone, benzene, butanol, ethanol, isobutanol, propanoic acid, propanol, 2-propanol and tert-butyl methyl ether. The behaviour of the total VOCs (tVOCs) intensity during the period of analysis and the relative variation between consecutive months were studied. It was observed that the overall trend of tVOCs closely mirrored the variation of air temperature throughout the year suggesting their strong correlation. The results obtained from this study demonstrate the high quality and relevance of the data, highlighting the suitability of GC-IMS for <i>in situ</i> long-term air quality assessment in indoor environments and, consequently, for identifying potential health risks for the human organism in both short-term and long-term exposure scenarios.</p>","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 4","pages":"231-239"},"PeriodicalIF":1.3,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10466997/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10498782","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Corrigendum.","authors":"","doi":"10.1177/14690667231170709","DOIUrl":"https://doi.org/10.1177/14690667231170709","url":null,"abstract":"Publication Note Due to an administrative error the article, ‘Mass spectrometric detection of ion pairs containing rigid copper clusters and weakly coordinating counter ions using liquid injection field desorption/ionisation’ by Julia Taubert, Matthias Vogt, and Robert Langer, intended for publication in the Special Issue ‘Liquid Injection Field Desorption Ionization (LIFDI) Mass Spectrometry (MS)’, was inadvertently missed to be included in the issue.","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 3","pages":"207"},"PeriodicalIF":1.3,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10330966/pdf/10.1177_14690667231170709.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10146505","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A HPLC-MS/MS method for the determination of Nadolol in rat plasma: Development, validation, and application to pharmacokinetic study.","authors":"Narasimha Kanjarla,&nbsp;Bhuvanachandra Pasupuleti,&nbsp;Narender Boggula,&nbsp;Praveen K Kusuma,&nbsp;Daniel Kothapally,&nbsp;Vamshikrishna Gone,&nbsp;Gangarapu Kiran","doi":"10.1177/14690667231179569","DOIUrl":"https://doi.org/10.1177/14690667231179569","url":null,"abstract":"<p><p>A sensitive validated method has been developed for the quantification of Nadolol in rat plasma by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) using deuterated Nadolol (Nadolol D9) as internal standard (IS). The liquid-liquid extraction method using ethyl acetate was employed for the sample pretreatment. The separation was achieved on the Agilent Zorbax XDB C18 column (150  mm  ×  4.6  mm ID., 3.5  μm). The column temperature was controlled at 30°C. The components were eluted by using mobile phase A (10  mM ammonium formate) and mobile phase B (acetonitrile) in the ratio of 20:80  v/v with a flow rate of 0.5  mL/min. And 15  μL aliquot was injected in an isocratic elution mode with a total run time of 2.5  min. The multiple reactions monitoring transitions, m/z 310.20/254.10 for Nadolol and IS 319.20/255.00 were selected to achieve high selective analysis. The method exhibited great selectivity and linearity over the concentration range of 6 to 3000  ng/mL. The lower limit of quantification was found to be 6  ng/mL. The developed method proved acceptable results on selectivity, sensitivity, precision, accuracy, and stability studies as per Food and Drug Administration guidelines. This HPLC-MS/MS assay was successfully applied to get the pharmacokinetics parameters in rat plasma.</p>","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 3","pages":"170-180"},"PeriodicalIF":1.3,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9967603","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Measurement of vitamin K and its derivatives in human plasma through enzyme-assisted liquid chromatography-tandem mass spectrometry assay.","authors":"Metin Demirel,&nbsp;Sahabettin Selek","doi":"10.1177/14690667231183046","DOIUrl":"https://doi.org/10.1177/14690667231183046","url":null,"abstract":"<p><p>Vitamin K is an essential lipophilic vitamin that acts as a coenzyme in several metabolic pathways. Accurate measurement of apolar metabolites transported by lipoproteins in serum matrices requires high-recovery extractions of vitamin K and its derivatives following standardized protocols. Conventionally developed methods in this field have predominantly employed solid-phase extraction for the measurement of vitamin K and its derivatives. In this study, our objective was to develop an enzyme-assisted extraction method for the precise measurement of vitamin K and its derivatives. Our methodology involved mixing 450 µL of serum samples with 50 µL of an internal standard and 50 µL of a lipase enzyme solution. Following vortexing, the mixture was incubated at 37°C for 15 min to activate the enzymes. The enzyme reaction was subsequently quenched with a mixture of 250 µL of methanol and 1 mL of hexane, followed by centrifugation at 12,000 <i>g</i> for 5 min. The upper phase was collected, concentrated using a concentrator device, and dissolved in a 100 µL solution of methanol/acetone/isopropanol (7:1:1, v/v/v) for analysis. Spectrum analysis was performed using the open-source MZmine 3 software, and a reference interval was established using the Python programming language on the Google Colab platform. The developed method for measuring vitamin K and its derivatives exhibited limit of detection and limit of quantitation values of 0.005 and 0.01 ng/mL, respectively. In conclusion, our study presents a precise and reliable method for the measurement of vitamin K and its derivatives using enzyme-assisted extraction.</p>","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 3","pages":"200-206"},"PeriodicalIF":1.3,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10047944","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Dynamic changes of serum metabolite profiling in septic mice based on high performance liquid chromatography of quadrupole time of flight mass spectrometry analysis.","authors":"Shutong Li,&nbsp;Qi Zeng,&nbsp;Shentang Li,&nbsp;Yarong Liu,&nbsp;Yang Feng,&nbsp;Fang Chen,&nbsp;Lianhong Zou,&nbsp;Xiehong Liu,&nbsp;Yanjuan Liu,&nbsp;Yu Jiang","doi":"10.1177/14690667231179565","DOIUrl":"https://doi.org/10.1177/14690667231179565","url":null,"abstract":"<p><p>The objective of this study is to gain insights into the underlying metabolic transformations that occurred during the whole progression of cecal ligation and puncture (CLP)-induced sepsis, thus providing new targets for its treatment. High-performance liquid chromatography of quadrupole time of flight mass spectrometry (HPLC-Q-TOF-MS/MS) combined with multivariate statistical techniques was used to detect the s in serum from septic mice. Fifty male mice were divided into two groups, including the sham group (<i>n</i> = 7) and the CLP-induced sepsis group (<i>n</i> = 43). Animals were sacrificed at 1, 3, 5, and 7 days post-CLP and then serum were collected for metabolomic analysis. Multivariate regression analysis was carried out through MetaboAnalyst 5.0, including principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA), to identify the s and screen out the related differential metabolites. Besides, the KEGG pathway analysis was used to analyze the related metabolic pathways in which the identified metabolites were involved. Based on the fold change (FC > 2.0 or <0.5), variable important in projection (VIP > 1.2), and <i>P</i> value (<i>P</i> < 0.05), we found 26, 17, 21, and 17 metabolites in septic mice at 1, 3, 5, and 7 days post-CLP, respectively, compared with that of the sham group. The PCA and PLS-DA pattern recognition showed a cluster-type distribution between the sham group and the CLP group. Dysregulated amino acid metabolism, as well as disturbed nucleotide metabolism, is observed. Several important metabolic pathways were identified between the sham group and the CLP group. Among them, phenylalanine metabolism, phenylalanine, tyrosine, and tryptophan biosynthesis showed striking at day 1 post-CLP. At day 3, phenylalanine, tyrosine, and tryptophan biosynthesis changed significantly. However, as the disease process, only pyrimidine metabolism showed the most significant alternation, compared to the sham group. Several differential metabolites were identified in the CLP group compared with that of the sham group and they were presented with dynamic alternation at different time points post-CLP, indicating metabolic disturbance occurred throughout the whole sepsis progression.</p>","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 3","pages":"159-169"},"PeriodicalIF":1.3,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10067019","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Gas chromatography-mass spectrometric determination of bisphenol residues by dispersive solid phase extraction followed by activated carbon spheres cleanup from fish feed samples.","authors":"Kalpana Talari,&nbsp;Sai Krishna Ganji,&nbsp;Raja Rajeswari Tiruveedula","doi":"10.1177/14690667231174446","DOIUrl":"https://doi.org/10.1177/14690667231174446","url":null,"abstract":"<p><p>Bisphenols are known endocrine disruptors commonly utilized in food packaging and storage materials, which frequently come into touch with multiple food products packed in them. The bisphenols in fish feed and other feed materials for aquatic organisms are harmful. The consumption of such marine foods is hazardous. Hence, the feed of aquatic products needs to be verified for the presence of bisphenols. The present study was focused on developing and validating a rapid, selective, and sensitive method to quantify 11 bisphenols from the fish feed with dispersive solid-phase extraction, which was cleaned by an optimized amount of activated carbon spheres and silylated by N,O-bis(trimethylsilyl)trifluoro acetamide and analyzed by gas chromatography-mass spectrometry. The new method was rigorously tested and verified after carefully tuning various parameters affecting analyte recovery. Limit of detection (LOD) were set at 0.5-5 ng/g and limit of quantification (LOQ) at 1-10 ng/g, respectively, resulting in 95-114% recoveries. Interday and intraday precisions in terms of relative standard deviation were found to be less than 11%. The proposed approach was effectively applied in floating and sinking fish feeds. The obtained results showed that higher concentration of bisphenol A, followed by bisphenol TMC, and bisphenol M at a concentration of 256.10, 159.01, and 168.82 ng/g in floating feed and 88.04, 200.79, and 98.03 ng/g in sinking feed samples, respectively.</p>","PeriodicalId":12007,"journal":{"name":"European Journal of Mass Spectrometry","volume":"29 3","pages":"181-191"},"PeriodicalIF":1.3,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10047448","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}