10,862 results match your criteria fragment ions

Discrimination of CBD-, THC- and CBC-type acid cannabinoids through diagnostic ions by UHPLC-HR-MS/MS in negative ion mode.

J Pharm Biomed Anal 2021 May 5;201:114125. Epub 2021 May 5.

Department of Environmental, Biological and Pharmaceutical Sciences and Technologies, University of Campania "Luigi Vanvitelli", Via Vivaldi 43, I-81100, Caserta, Italy. Electronic address:

The interest in industrial hemp-based products and by-products to be utilized in food and nutraceutical sector is strictly linked to the demand for improved analytical methods to rapidly discriminate acid phytocannabinoid isomers. Indeed, the differentiation of acid phytocannabinoids, also named pre-cannabinoids, is not properly exploited and valued until now, and it is challenging. Herein, using high-resolution MS/MS, the most common pre-cannabinoids with the resorcinol core linked to the alkyl five carbons chain were deeply investigated in terms of their reactivity to collision-induced dissociation, gaining key data on the integrated energy framework of their dissociation pathway. Read More

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Visualizing Lithiation of Graphite Composite Anodes in All-Solid-State Batteries Using Time-of-Flight Secondary Ion Mass Spectrometry.

J Phys Chem Lett 2021 May 11:4623-4627. Epub 2021 May 11.

Applied Materials Technology Center, Technology Division, Panasonic Corporation, 3-1-1 Yagumo-nakamachi, Moriguchi, Osaka 570-8501, Japan.

A fundamental understanding of lithiation dynamics in composite electrodes is essential for the development of all-solid-state batteries with high capacity and rate capability. However, a comprehensive methodology to monitor the time evolution of lithiation in a composite electrode has not been fully established because of the limitations of the characterization techniques currently employed. In this study, we demonstrate the visualization of the transient distribution of Li in composite graphite anodes during cell operation using time-of-flight secondary ion mass spectrometry. Read More

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Mass Spectrometry-Based Shotgun Lipidomics Using Charge-Switch Derivatization for Analysis of Complex Long-Chain Fatty Acids.

Methods Mol Biol 2021 ;2306:93-103

Mass Spectrometry Resource, Division of Endocrinology, Metabolism, and Lipid Research, Department of Medicine, Washington University School of Medicine, St. Louis, MO, USA.

Charge-switch derivatization to convert long-chain fatty acids (LCFAs) to their N-(4-aminomethylphenyl) pyridinium (AMPP) derivatives (FA-AMPP derivative) drastically increases their sensitivity (>10) detected by electrospray ionization (ESI) or matrix assisted laser desorption ionization (MALDI). Lipidomic analyses of the FA-AMPP derivatives by ESI combined with CID tandem mass spectrometry (MS), or by MALDI-TOF/TOF affords unambiguous structural characterization of LCFAs, including many unusual microbial LCFAs that contain various functional groups such as methyl, hydroxyl, cyclopropyl, and double bond(s). The ease of preparation of the FA-AMPP derivatives, the tremendous gain in sensitivity after derivatization, and more importantly, the readily recognizable product ion spectra that contain rich structurally informative fragment ions for locating functional groups make this method one of the most powerful techniques for LCFA identification and quantification. Read More

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January 2021

Comprehensive Structural Characterization of Lipids by Coupling Paternò-Büchi Reaction and Tandem Mass Spectrometry.

Methods Mol Biol 2021 ;2306:53-60

State Key Laboratory of Precision Measurement Technology and Instruments, Department of Precision Instrument, Tsinghua University, Beijing, China.

Since the invention of soft ionization methods, in particular electrospray ionization (ESI), mass spectrometry (MS) has become the method of choice for both qualitative and quantitative analysis of lipids from complex samples. A large number of lipids can be readily detected from a single mass spectrum free from molecular fragmentation that may complicate spectral interpretation. This has been the driving force for MS to play a predominant role in lipidomics. Read More

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January 2021

Targeted Protein Quantification Using Parallel Reaction Monitoring (PRM).

Methods Mol Biol 2021 ;2228:145-157

Medizinisches Proteom-Center (MPC), Ruhr-Universität Bochum, Bochum, Germany.

Targeted proteomics represents an efficient method to quantify proteins of interest with high sensitivity and accuracy. Targeted approaches were first established for triple quadrupole instruments, but the emergence of hybrid instruments allowing for high-resolution and accurate-mass measurements of MS/MS fragment ions enabled the development of parallel reaction monitoring (PRM). In PRM analysis, specific peptides are measured as representatives of proteins in complex samples, with the full product ion spectra being acquired, allowing for identification and quantification of the peptides. Read More

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January 2021

An Approach for Triplex-IPTL.

Methods Mol Biol 2021 ;2228:133-144

Department of Biosciences, University of Oslo, Oslo, Norway.

Isobaric peptide termini labeling (IPTL) is an approach for quantitative proteomics based on crosswise isotopic labeling of peptides at the N- and C-terminus. The labeling reagents are chosen in isotopic variations that the resulting mass of all labels per peptide is isobaric, but the individual label on each peptide terminus is different. Therefore, the quantitative difference of the peptide signal can be determined by the fragment ions of the corresponding MS2 spectra. Read More

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January 2021

In situ Detection of Fatty Acid C=C Positional Isomers by Coupling On-tissue mCPBA Epoxidation with IR-MALDESI Mass Spectrometry.

Rapid Commun Mass Spectrom 2021 May 3:e9119. Epub 2021 May 3.

FTMS Laboratory for Human Health Research, Department of Chemistry, North Carolina State University, Raleigh, NC, 27695.

Rationale: Unsaturated fatty acids (UFAs) play vital roles in regulating cellular functions. In-depth structural characterization of UFAs such as localizing carbon-carbon double bonds is fundamentally important but poses considerable challenges in mass spectrometry (MS) given that the most widely accessible ion activation method, low-energy collision-induced dissociation, primarily generates uninformative fragments (e.g. Read More

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Investigation of the molecular structure complexity of dissolved organic matter by UPLC-orbitrap MS/MS.

Talanta 2021 Aug 20;230:122320. Epub 2021 Mar 20.

Center of Excellence for Environmental Safety and Biological Effects, Beijing Key Laboratory for Green Catalysis and Separation, Department of Chemistry and Biology, Beijing University of Technology, Beijing, 100124, China. Electronic address:

The complex natural organic matter of the Suwannee River fulvic acid (SRFA) standard was analyzed by online reversed-phase chromatography with Orbitrap MS/MS using collision-induced dissociation (CID). The number of isobars per nominal mass could be reduced to a single dominantly abundant species in a chromatographic run, sharing some ions with signals having the identical molecular formula in adjacent chromatographic segments and later serving as a precursor ion for fragmentation. A very large proportion of the same fragment ions existed in adjacent chromatographic fractions. Read More

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The study of the chromatographic behavior and a mass spectrometric approach to differentiating the diastereomer pair of the β-O-4 lignin dimer series.

Anal Bioanal Chem 2021 May 2. Epub 2021 May 2.

Department of Chemistry, University of Kentucky, Lexington, KY, 40506, USA.

Lignin and lignans are natural products found in plant cell walls. Lignin research has historically focused on lignin degradation techniques in the hope of converting lignin into useful aromatic carbon feedstocks. In contrast, investigations of lignans existing as natural product dimers, have been focused on thier interesting biological activities. Read More

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Catechol-Containing Schiff Bases on Thiacalixarene: Synthesis, Copper (II) Recognition, and Formation of Organic-Inorganic Copper-Based Materials.

Molecules 2021 Apr 17;26(8). Epub 2021 Apr 17.

A.M. Butlerov' Chemistry Institute, Kazan Federal University, 18 Kremlevskaya Street, 420008 Kazan, Russia.

For the first time, a series of catechol-containing Schiff bases, tetrasubstituted at the lower rim thiacalix[4]arene derivatives in three stereoisomeric forms, , , and , were synthesized. The structure of the obtained compounds was proved by modern physical methods, such as NMR, IR spectroscopy, and HRMS. Selective recognition (K difference by three orders of magnitude) of copper (II) cation in the series of d-metal cations (Cu, Ni, Co, Zn) was shown by UV-vis spectroscopy. Read More

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Mono- and Binuclear Copper(II) and Nickel(II) Complexes with the 3,6-Bis(picolylamino)-1,2,4,5-Tetrazine Ligand.

Molecules 2021 Apr 7;26(8). Epub 2021 Apr 7.

Univ Angers, CNRS, MOLTECH-Anjou, SFR MATRIX, F-49000 Angers, France.

Four new compounds of formulas [Cu(hfac)(L)] (), [Ni(hfac)(L)] (), [{Cu(hfac)}(µ-L)]·2CHOH () and [{Ni(hfac)}(µ-L)]·2CHCN () [Hhfac = hexafluoroacetylacetone and L = 3,6-bis(picolylamino)-1,2,4,5-tetrazine] have been prepared and their structures determined by X-ray diffraction on single crystals. Compounds and are isostructural mononuclear complexes where the metal ions [copper(II) () and nickel(II) ()] are six-coordinated in distorted octahedral MNO surroundings which are built by two bidentate hfac ligands plus another bidentate L molecule. This last ligand coordinates to the metal ions through the nitrogen atoms of the picolylamine fragment. Read More

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Gangliosides of Human Glioblastoma Multiforme: A Comprehensive Mapping and Structural Analysis by Ion Mobility Tandem Mass Spectrometry.

J Am Soc Mass Spectrom 2021 May 26;32(5):1249-1257. Epub 2021 Apr 26.

Department of Condensed Matter, National Institute for Research and Development in Electrochemistry and Condensed Matter, 300224, Timisoara, Romania.

Glioblastoma multiforme (GBM), a malignant, highly aggressive, grade IV brain tumor, which rapidly infiltrates into the nearby tissue, has drawn a significant amount of attention because of its poor prognosis and the limited treatment options available. In GBM, nearly all tumor cells exhibit aberrant cell-surface glycosylation patterns due to the alteration of their biosynthesis or postsynthesis modification process. Since gangliosides (GGs) are acknowledged as tumor-associated antigens, we have carried out here a comprehensive profiling of native ganglioside mixtures extracted and purified from GBM specimens. Read More

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Fragmentation mechanisms of protonated cyclodextrins in tandem mass spectrometry.

Carbohydr Res 2021 Apr 20;504:108316. Epub 2021 Apr 20.

Department of Chemistry, Biochemistry and Pharmaceutical Sciences, University of Bern, Freiestrasse 3, CH-3012 Bern, Switzerland. Electronic address:

Tandem mass spectrometry has found widespread application as a powerful tool for the characterization of linear and branched oligosaccharides. Though the technique has been applied to the analysis of cyclic oligosaccharides as well, the underlying fragmentation mechanisms have hardly been investigated. This study focuses on the mechanistic aspects of the gas-phase dissociation of protonated β-cyclodextrins. Read More

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Intramolecular CH-migration-controlled cation reactions in the VUV photochemistry of 2-methyl-3-buten-2-ol investigated by synchrotron photoionization mass spectrometry and theoretical calculations.

Phys Chem Chem Phys 2021 May;23(17):10456-10467

National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei, Anhui 230029, P. R. China.

2-Methyl-3-buten-2-ol (MBO232) is a biogenic volatile organic compound (BVOC), and has a large percentage of emission into the atmosphere. The vacuum ultraviolet (VUV) photochemistry of BVOCs is of great importance for atmospheric chemistry. Studies have been carried out on several BVOCs but have not extended to MBO232. Read More

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Experimental and theoretical assessment of protonated Hoogsteen 9-methylguanine-1-methylcytosine base-pair dissociation: kinetics within a statistical reaction framework.

Phys Chem Chem Phys 2021 Apr;23(15):9365-9380

Department of Chemistry and Biochemistry, Queens College of the City University of New York, 65-30 Kissena Blvd., Queens, NY 11367, USA. and Ph.D. Program in Chemistry, The Graduate Center of the City University of New York, 365 5th Ave., New York, NY 10016, USA.

We investigated the collision-induced dissociation (CID) reactions of a protonated Hoogsteen 9-methylguanine-1-methylcytosine base pair (HG-[9MG·1MC + H]+), which aims to address the mystery of the literature reported "anomaly" in product ion distributions and compare the kinetics of a Hoogsteen base pair with its Watson-Crick isomer WC-[9MG·1MC + H]+ (reported recently by Sun et al.; Phys. Chem. Read More

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Suspect screening and targeted analysis of acyl coenzyme A thioesters in bacterial cultures using a high-resolution tribrid mass spectrometer.

Anal Bioanal Chem 2021 Apr 21. Epub 2021 Apr 21.

Organic Geochemistry, Carl von Ossietzky University Oldenburg, 26129, Oldenburg, Germany.

Analysis of acyl coenzyme A thioesters (acyl-CoAs) is crucial in the investigation of a wide range of biochemical reactions and paves the way to fully understand the concerned metabolic pathways and their superimposed networks. We developed two methods for suspect screening of acyl-CoAs in bacterial cultures using a high-resolution Orbitrap Fusion tribrid mass spectrometer. The methods rely on specific fragmentation patterns of the target compounds, which originate from the coenzyme A moiety. Read More

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Water structure around a left-handed Z-DNA fragment analyzed by cryo neutron crystallography.

Nucleic Acids Res 2021 May;49(8):4782-4792

Department of Biochemistry and Center for Structural Biology, Vanderbilt University, School of Medicine, Nashville, TN 37232, USA.

Even in high-quality X-ray crystal structures of oligonucleotides determined at a resolution of 1 Å or higher, the orientations of first-shell water molecules remain unclear. We used cryo neutron crystallography to gain insight into the H-bonding patterns of water molecules around the left-handed Z-DNA duplex [d(CGCGCG)]2. The neutron density visualized at 1. Read More

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Valence Photoionization and Energetics of Vanillin, a Sustainable Feedstock Candidate.

J Phys Chem A 2021 Apr 19;125(16):3327-3340. Epub 2021 Apr 19.

Paul Scherrer Institute, 5232 Villigen, Switzerland.

We studied the valence photoionization of vanillin by photoelectron photoion coincidence spectroscopy in the 8.20-19.80 eV photon energy range. Read More

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A chemometric strategy for accurately identifying illegal additive compounds in health foods by using ultra-high-performance liquid chromatography coupled to high resolution mass spectrometry.

Anal Methods 2021 04 23;13(14):1731-1739. Epub 2021 Mar 23.

College of Pharmacy, Ningxia Medical University, Yinchuan 750004, China.

The accurate identification of unknown illegal additive compounds in complex health foods continues to be a challenging task in routine analysis, because massive false positive results can be screened with ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry-based untargeted techniques and must be manually filtered out. To address this problem, we developed a chemometric-based strategy, in which data analysis was first performed by using XCMS, MS-DIAL, Mzmine2, and AntDAS2, to select those that provided acceptable results to extract common features (CFs), which can be detected by all of the selected methods. Then, CFs whose contents were significantly higher in the suspected illegal additive group were screened. Read More

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Ro-vibrational Distribution of NO Dissociated from NO Ions in the aB and bA States: A Slow "Impulsive" Dissociation Example Revealed from Threshold Photoelectron-Photoion Coincidence Imaging.

J Phys Chem A 2021 Apr 16;125(16):3316-3326. Epub 2021 Apr 16.

Hefei National Laboratory for Physical Sciences at the Microscale, Department of Chemical Physics, University of Science and Technology of China, Hefei 230026, China.

To clarify the contentions about dissociative photoionization mechanism of nitrogen dioxide via the aB and bA ionic states, a new threshold photoelectron-photoion coincidence (TPEPICO) velocity imaging has been conducted in the 12.8-14.0 eV energy range at the Hefei Light Source. Read More

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High-Coverage Screening of Sulfonamide Metabolites in Goat Milk by Magnetic Doped S Graphene Combined with Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometry.

J Agric Food Chem 2021 Apr 16;69(16):4755-4765. Epub 2021 Apr 16.

School of Food and Biological Engineering, Shaanxi University of Science & Technology, Xi'an 710021, China.

Currently, there are more than 1000 varieties of synthetic sulfonamides universally used as antibiotics causing severe results of potential carcinogenicity and drug resistance for human health due to excessive residue of animal-derived food. A facile and novel approach for untargeted screening of sulfonamides (SAs) and metabolites was proposed based on magnetic solid-phase extraction-ultrahigh-performance liquid chromatography-tandem high-resolution mass spectrometry (MSPE-UHPLC-HRMS). Compared with QuEChERS without the clean-up procedure and SPE in terms of matrix effect and absolute recovery, magnetic doped S graphene (S-doping level: 2. Read More

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Formation of covalently bound CH upon electron-impact ionization of acetylene dimer.

J Chem Phys 2021 Apr;154(14):144301

MOE Key Laboratory for Nonequilibrium Synthesis and Modulation of Condensed Matter, School of Physics, Xi'an Jiaotong University, Xi'an 710049, China.

We investigate the formation mechanisms of covalently bound CH cations from direct ionization of hydrogen bonded dimers of acetylene molecules through fragment ion and electron coincident momentum spectroscopy and quantum chemistry calculations. The measurements of momenta and energies of two outgoing electrons and one ion in triple-coincidence allow us to assign the ionization channels associated with different ionic fragments. The measured binding energy spectra show that the formation of CH can be attributed to the ionization of the outermost 1π orbital of acetylene. Read More

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Sensitive Immunopeptidomics by Leveraging Available Large-Scale Multi-HLA Spectral Libraries, Data-Independent Acquisition, and MS/MS Prediction.

Mol Cell Proteomics 2021 Apr 9;20:100080. Epub 2021 Apr 9.

Department of Oncology, Ludwig Institute for Cancer Research Lausanne, Lausanne University Hospital and the University of Lausanne, Lausanne, Switzerland. Electronic address:

Mass spectrometry (MS) is the state-of-the-art methodology for capturing the breadth and depth of the immunopeptidome across human leukocyte antigen (HLA) allotypes and cell types. The majority of studies in the immunopeptidomics field are discovery driven. Hence, data-dependent tandem MS (MS/MS) acquisition (DDA) is widely used, as it generates high-quality references of peptide fingerprints. Read More

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Increasing Top-Down Mass Spectrometry Sequence Coverage by an Order of Magnitude through Optimized Internal Fragment Generation and Assignment.

Anal Chem 2021 04 12;93(16):6355-6362. Epub 2021 Apr 12.

Department of Chemistry and Chemical Biology, Northeastern University, Boston, Massachusetts 02115, United States.

A major limitation of intact protein fragmentation is the lack of sequence coverage within proteins' interiors. We show that collisionally activated dissociation (CAD) produces extensive internal fragmentation within proteins' interiors that fill the existing gaps in sequence coverage, including disulfide loop regions that cannot be characterized using terminal fragments. A barrier to the adoption of internal fragments is the lack of methods for their generation and assignment. Read More

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Development and validation of a simultaneous analytical method for non-steroidal therapeutic compounds in cosmetics using liquid chromatography-tandem mass spectrometry.

J Sep Sci 2021 Apr 9. Epub 2021 Apr 9.

Center for Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong Health Technology Administration Complex, Cheongju-si, Chungcheongbuk-do, Republic of Korea.

Atopic dermatitis is a typical chronic inflammatory skin disease that affects all age groups and requires basic skin care for treatment. Anti-inflammatory and antiallergy steroids are the most frequently used treatments but they are limited due to their side effects caused by a weakening of the immune system. Many consumers focus on performance as a criterion for selecting cosmetics. Read More

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Components identification and isomers differentiation in pigeon pea (Cajanus cajan L.) leaves by LC-MS.

J Sep Sci 2021 Apr 8. Epub 2021 Apr 8.

Key Laboratory for Green Pharmaceutical Technologies and Related Equipment of Ministry of Education, College of Pharmaceutical Sciences, Zhejiang University of Technology, Hangzhou, 310014, China.

A valid and reliable method based on ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry using electrospray ionization was established to identify chemical constituents in the ethanol extract of pigeon pea leaves. A total of 58 compounds were detected both in positive and negative modes. Among them, 42 compounds including 16 flavones, 1 flavonol, 5 flavanones, 9 isoflavones, 1 coumarin, 1 lactone, 6 stilbenes, 2 chalcones and 1 other compound were unambiguously identified or tentatively assigned in view of the retention time, the molecular formula as well as the fragmentation patterns. Read More

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Pharmacokinetics, bioavailability and metabolism of CC-92480 in rat by liquid chromatography combined with electrospray ionization tandem mass spectrometry.

Weili You Jie Pang

Biomed Chromatogr 2021 Apr 8:e5139. Epub 2021 Apr 8.

Department of Pharmacy, The Affiliated Lianyungang Hospital of Xuzhou Medical University/The First People's Hospital of Lianyungang, Lianyungang, Jiangsu Province, China.

CC-92480 is a cereblon E3 ubiquitin ligase modulating drug with potent antimyeloma activity. In this study, we developed a sensitive UHPLC-MS/MS method for the determination of CC-92480 in rat plasma. The plasma samples were prepared with acetonitrile and the samples were then separated on an Acquity BEH C column (2. Read More

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Novel Strategy for Untargeted Chiral Metabolomics using Liquid Chromatography-High Resolution Tandem Mass Spectrometry.

Anal Chem 2021 04 5;93(14):5805-5814. Epub 2021 Apr 5.

Department of Nutritional Sciences, College of Natural Sciences, The University of Texas at Austin, Austin, Texas 78712, United States.

Stereospecific recognition of metabolites plays a significant role in the detection of potential disease biomarkers thereby providing new insights in diagnosis and prognosis. D-Hdroxy/amino acids are recognized as potential biomarkers in several metabolic disorders. Despite continuous advances in metabolomics technologies, the simultaneous measurement of different classes of enantiomeric metabolites in a single analytical run remains challenging. Read More

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Rapid screening of 70 colorants in dyeable foods by using ultra-high-performance liquid chromatography-hybrid quadrupole-Orbitrap mass spectrometry with customized accurate-mass database and mass spectral library.

Food Chem 2021 Sep 22;356:129643. Epub 2021 Mar 22.

Chengdu Institute of Biology, Chinese Academy of Sciences, No. 93 South Keyuan Road, Gaoxin Distinct, Chengdu 610041, China. Electronic address:

A rapid screening method of 70 colorants for regulatory control in dyeable foods was established using ultra-high-performance liquid chromatography-hybrid quadrupole-Orbitrap mass spectrometry (UHPLC-Q/Orbitrap MS) with customized accurate-mass database and mass spectral library. A rapid, high-throughput, and simple sample pretreatment condition with low reagent consumption and high recovery was developed on the basis of ultrasound-assisted extraction and dispersion solid-phase extraction. Rapid screening was conducted by comparing the experimentally measured exact mass of the parent and fragment ions, the isotope pattern, and the retention time with the accurate-mass database and by matching the acquired MS/MS spectra against the mass spectral library. Read More

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September 2021

EPIP-Evoked Modifications of Redox, Lipid, and Pectin Homeostasis in the Abscission Zone of Lupine Flowers.

Int J Mol Sci 2021 Mar 16;22(6). Epub 2021 Mar 16.

Department of Plant Physiology and Biotechnology, Nicolaus Copernicus University, 1 Lwowska Street, 87-100 Toruń, Poland.

Yellow lupine is a great model for abscission-related research given that excessive flower abortion reduces its yield. It has been previously shown that the EPIP peptide, a fragment of LlIDL (INFLORESCENCE DEFICIENT IN ABSCISSION) amino-acid sequence, is a sufficient molecule to induce flower abortion, however, the question remains: What are the exact changes evoked by this peptide locally in abscission zone (AZ) cells? Therefore, we used EPIP peptide to monitor specific modifications accompanied by early steps of flower abscission directly in the AZ. EPIP stimulates the downstream elements of the pathway- and MITOGEN-ACTIVATED PROTEIN KINASE6 and induces cellular symptoms indicating AZ activation. Read More

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