Selectivity of the confirmation of identity in liquid chromatography (tandem) mass spectrometry using Q-Orbitrap instrumentation was assessed using different acquisition modes based on a representative experimental data set constructed from 108 samples, including six different matrix extracts and containing over 100 analytes each. Single stage full scan, all ion fragmentation, and product ion scanning were applied. By generating reconstructed ion chromatograms using unit mass window in targeted MS(2), selected reaction monitoring (SRM), regularly applied using triple-quadrupole instruments, was mimicked. This facilitated the comparison of single stage full scan, all ion fragmentation, (mimicked) SRM, and product ion scanning applying a mass window down to 1 ppm. Single factor Analysis of Variance was carried out on the variance (s(2)) of the mass error to determine which factors and interactions are significant parameters with respect to selectivity. We conclude that selectivity is related to the target compound (mainly the mass defect), the matrix, sample clean-up, concentration, and mass resolution. Selectivity of the different instrumental configurations was quantified by counting the number of interfering peaks observed in the chromatograms. We conclude that precursor ion selection significantly contributes to selectivity: monitoring of a single product ion at high mass accuracy with a 1 Da precursor ion window proved to be equally selective or better to monitoring two transition products in mimicked SRM. In contrast, monitoring a single fragment in all ion fragmentation mode results in significantly lower selectivity versus mimicked SRM. After a thorough inter-laboratory evaluation study, the results of this study can be used for a critical reassessment of the current identification points system and contribute to the next generation of evidence-based and robust performance criteria in residue analysis and sports doping.
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http://dx.doi.org/10.1007/s13361-014-1021-x | DOI Listing |
Mass Spectrom Rev
January 2025
Department of Chemistry, University of Texas at Austin, Austin, Texas, USA.
Mass spectrometry (MS) has become a critical tool in the characterization of covalently modified nucleic acids. Well-developed bottom-up approaches, where nucleic acids are digested with an endonuclease and the resulting oligonucleotides are separated before MS and MS/MS analysis, provide substantial insight into modified nucleotides in biological and synthetic nucleic. Top-down MS presents an alternative approach where the entire nucleic acid molecule is introduced to the mass spectrometer intact and then fragmented by MS/MS.
View Article and Find Full Text PDFMolecules
December 2024
Centre for Research University Services (CeSAR), Università degli Studi di Cagliari, S.S. 554 Bivio per Sestu, 09042 Monserrato, Italy.
2,8-Dithia-5-aza-2,6-pyridinophane () has been used as a receptor unit in the construction of the conjugated redox chemosensor 5-ferrocenylmethyl-2,8-dithia-5-aza-2,6-pyridinophane (). In order to further explore the coordination chemistry of , and comparatively, that of its structural analogue 2,11-dithia-5,8-diaza-2,6-pyridinophane (), featuring two secondary nitrogen atoms in the macrocyclic unit, the crystal structures of the new synthesised complexes [Pb()(ClO)]·½CHCN, [Cu()](ClO)·CHCN and [Cd()(NO)]NO were determined by X-ray diffraction analysis. The electrochemical response of towards the metal ions Cu, Zn, Cd, Hg, and Pb was investigated by cyclic voltammetry (CV) in CHCl/CHCN 0.
View Article and Find Full Text PDFJ Pharm Biomed Anal
January 2025
Department of Pharmaceutical Analysis, School of Pharmacy, Guizhou Medical University, Gui'an New District, Guizhou 561113, PR China. Electronic address:
Dendrobine is a sesquiterpene alkaloid primarily used in the treatment of inflammatory diseases, immune system disorders, and conditions related to oxidative stress. To understand the possible degradation pathways of dendrobine for its quality control, we conducted an in-depth investigation of its degradation products using forced degradation methods. The separation of dendrobine and its degradation products was achieved on a Shim-pack XR-ODS III (75 mm × 2 mm, 1.
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
January 2025
The First Clinical Medical College, Shandong University of Traditional Chinese Medicine, Jinan, 250355, PR China; Department of Pharmacy, Affiliated Hospital of Shandong University of Traditional Chinese Medicine, Jinan 250014, PR China. Electronic address:
The sensitive and accurate detection of copper ions is crucial for public health, medical research, and environmental monitoring. In this study, we developed a sensor based on template-assembly activation of the primer exchange reaction (PER) for the on-site detection of copper ions in blood. Copper ions triggered the assembly of two template fragments into a hairpin structure via a click-chemistry reaction, activating the PER.
View Article and Find Full Text PDFPlant Cell
January 2025
State Key Laboratory of Plant Environmental Resilience, China Agricultural University, Beijing 100193, China.
Salt stress causes ion toxicity in plant cells and limits plant growth and crop productivity. Sodium ions (Na+) are transported out of the cell and sequestered in the vacuole for detoxification under salt stress. The salt excretion system is controlled by the SALT OVERLY SENSITIVE (SOS) pathway, which consists of the calcium sensors SOS3 and SOS3-LIKE CALCIUM BINDING PROTEIN 8, the protein kinase SOS2, and the plasma membrane Na+/H+ antiporter SOS1.
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