Journal articles: 'LC-MS/MS and LC/HRMS'

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Millet, Aurélien, Nihel Khoudour, Pauline Bros, Dorothée Lebert, Guillaume Picard, Christelle Machon, François Goldwasser, Benoit Blanchet, and Jérôme Guitton. "Quantification of nivolumab in human plasma by LC-MS/HRMS and LC-MS/MS, comparison with ELISA." Talanta 224 (March 2021): 121889. http://dx.doi.org/10.1016/j.talanta.2020.121889.

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Klijnstra, Mirjam, and Arjen Gerssen. "A Sensitive LC-MS/MS Method for Palytoxin Using Lithium Cationization." Toxins 10, no. 12 (December 14, 2018): 537. http://dx.doi.org/10.3390/toxins10120537.

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Palytoxin (PlTX) and analogues are produced by certain dinoflagellates, sea anemones, corals and cyanobacteria. PlTX can accumulate in the food chain and when consumed it may cause intoxication with symptoms like myalgia, weakness, fever, nausea, and vomiting. The analysis of PlTXs is challenging, and because of the large molecular structure, it is difficult to develop a sensitive and selective liquid chromatography-mass spectrometry (LC-MS/MS) method. In this work, an LC-MS/MS method was developed to analyse PlTXs with use of lithium iodine and formic acid as additives in the mobile phase. For method development, initially, LC-hrMS was used to accurately determine the elemental composition of the precursor and product ions. The main adduct formed was [M + H + 2Li]3+. Fragments were identified with LC-hrMS and these were incorporated in the LC-MS/MS method. A method of 10 min was developed and a solid phase extraction clean-up procedure was optimised for shellfish matrix. The determined limits of detection were respectively 8 and 22 µg PlTX kg−1 for mussel and oyster matrix. Oysters gave a low recovery of approximately 50% for PlTX during extraction. The method was successfully in-house validated, repeatability had a relative standard deviation less than 20% (n = 5) at 30 µg PlTX kg−1 in mussel, cockle, and ensis, and at 60 µg PlTX kg−1 in oyster.

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Kintz, Pascal, Alice Ameline, Laurie Gheddar, and Jean‐Sébastien Raul. "Testing for GW501516 (cardarine) in human hair using LC/MS–MS and confirmation by LC/HRMS." Drug Testing and Analysis 12, no. 7 (April 25, 2020): 980–86. http://dx.doi.org/10.1002/dta.2802.

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Millet, Aurélien, Nihel Khoudour, Dorothée Lebert, Christelle Machon, Benjamin Terrier, Benoit Blanchet, and Jérôme Guitton. "Development, Validation, and Comparison of Two Mass Spectrometry Methods (LC-MS/HRMS and LC-MS/MS) for the Quantification of Rituximab in Human Plasma." Molecules 26, no. 5 (March 4, 2021): 1383. http://dx.doi.org/10.3390/molecules26051383.

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Rituximab is a chimeric immunoglobulin G1-kappa (IgG1κ) antibody targeting the CD20 antigen on B-lymphocytes. Its applications are various, such as for the treatment of chronic lymphoid leukemia or non-Hodgkin’s lymphoma in oncology, and it can also be used in the treatment of certain autoimmune diseases. Several studies support the interest in therapeutic drug monitoring to optimize dosing regimens of rituximab. Thus, two different laboratories have developed accurate and reproductive methods to quantify rituximab in human plasma: one using liquid chromatography quadripolar tandem mass spectrometer (LC-MS/MS) and the other, liquid chromatography orbitrap tandem mass spectrometer (LC-MS/HRMS). For both assays, quantification was based on albumin depletion or IgG-immunocapture, surrogate peptide analysis, and full-length stable isotope-labeled rituximab. With LC-MS/MS, the concentration range was from 5 to 500 µg/mL, the within- and between-run precisions were <8.5%, and the limit of quantitation was 5 µg/mL. With LC-MS/HRMS, the concentration range was from 10 to 200 µg/mL, the within- and between-run accuracy were <11.5%, and the limit of quantitation was 2 µg/mL. Rituximab plasma concentrations from 63 patients treated for vasculitis were compared. Bland–Altman analysis and Passing–Bablok regression showed the interchangeability between these two methods. Overall, these methods were robust and reliable and could be applied to routine clinical samples.

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Kotapati, Srikanth, Madhura Deshpande, Aarti Jashnani, Dharam Thakkar, Hongwu Xu, and Gavin Dollinger. "The role of ligand-binding assay and LC–MS in the bioanalysis of complex protein and oligonucleotide therapeutics." Bioanalysis 13, no. 11 (June 2021): 931–54. http://dx.doi.org/10.4155/bio-2021-0009.

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Ligand-binding assay (LBA) and LC–MS have been the preferred bioanalytical techniques for the quantitation and biotransformation assessment of various therapeutic modalities. This review provides an overview of the applications of LBA, LC–MS/MS and LC–HRMS for the bioanalysis of complex protein therapeutics including antibody–drug conjugates, fusion proteins and PEGylated proteins as well as oligonucleotide therapeutics. The strengths and limitations of LBA and LC–MS, along with some guidelines on the choice of appropriate bioanalytical technique(s) for the bioanalysis of these therapeutic modalities are presented. With the discovery of novel and more complex therapeutic modalities, there is an increased need for the biopharmaceutical industry to develop a comprehensive bioanalytical strategy integrating both LBA and LC–MS.

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Kryuchkov, Fedor, Alison Robertson, Elizabeth M. Mudge, Christopher O. Miles, Soetkien Van Gothem, and Silvio Uhlig. "Reductive Amination for LC–MS Signal Enhancement and Confirmation of the Presence of Caribbean Ciguatoxin-1 in Fish." Toxins 14, no. 6 (June 9, 2022): 399. http://dx.doi.org/10.3390/toxins14060399.

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Ciguatera poisoning is a global health concern caused by the consumption of seafood containing ciguatoxins (CTXs). Detection of CTXs poses significant analytical challenges due to their low abundance even in highly toxic fish, the diverse and in-part unclarified structures of many CTX congeners, and the lack of reference standards. Selective detection of CTXs requires methods such as liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) or high-resolution MS (LC–HRMS). While HRMS data can provide greatly improved resolution, it is typically less sensitive than targeted LC–MS/MS and does not reliably comply with the FDA guidance level of 0.1 µg/kg CTXs in fish tissue that was established for Caribbean CTX-1 (C-CTX-1). In this study, we provide a new chemical derivatization approach employing a fast and simple one-pot derivatization with Girard’s reagent T (GRT) that tags the C-56-ketone intermediate of the two equilibrating C-56 epimers of C-CTX-1 with a quaternary ammonium moiety. This derivatization improved the LC–MS/MS and LC–HRMS responses to C-CTX-1 by approximately 40- and 17-fold on average, respectively. These improvements in sensitivity to the GRT-derivative of C-CTX-1 are attributable to: the improved ionization efficiency caused by insertion of a quaternary ammonium ion; the absence of adduct-ions and water-loss peaks for the GRT derivative in the mass spectrometer, and; the prevention of on-column epimerization (at C-56 of C-CTX-1) by GRT derivatization, leading to much better chromatographic peak shapes. This C-CTX-1–GRT derivatization strategy mitigates many of the shortcomings of current LC–MS analyses for C-CTX-1 by improving instrument sensitivity, while at the same time adding selectivity due to the reactivity of GRT with ketones and aldehydes.

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Nguyen, D. D., F. Busetti, S. K. Johnson, and V. A. Solah. "Identification and quantification of native beta-casomorphins in Australian milk by LC–MS/MS and LC–HRMS." Journal of Food Composition and Analysis 44 (December 2015): 102–10. http://dx.doi.org/10.1016/j.jfca.2015.08.009.

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Qiu, Jiangbing, Elliott J. Wright, Krista Thomas, Aifeng Li, Pearse McCarron, and Daniel G. Beach. "Semiquantitation of Paralytic Shellfish Toxins by Hydrophilic Interaction Liquid Chromatography-Mass Spectrometry Using Relative Molar Response Factors." Toxins 12, no. 6 (June 16, 2020): 398. http://dx.doi.org/10.3390/toxins12060398.

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Paralytic shellfish toxins (PSTs) are a complex class of analogs of the potent neurotoxin saxitoxin (STX). Since calibration standards are not available for many PSTs, including C-11 hydroxyl analogs called M-toxins, accurate quantitation by liquid chromatography–mass spectrometry (LC-MS) can be challenging. In the absence of standards, PSTs are often semiquantitated using standards of a different analog (e.g., STX), an approach with a high degree of uncertainty due to the highly variable sensitivity between analytes in electrospray ionization. Here, relative molar response factors (RMRs) were investigated for a broad range of PSTs using common LC-MS approaches in order to improve the quantitation of PSTs for which standards are unavailable. First, several M-toxins (M1-M6, M9 and dcM6) were semipurified from shellfish using preparative gel filtration chromatography and quantitated using LC-charged aerosol detection (LC-CAD). The RMRs of PST certified reference materials (CRMs) and M-toxins were then determined using selective reaction monitoring LC-MS/MS and full scan LC-high-resolution MS (LC-HRMS) methods in positive and negative electrospray ionization. In general, RMRs for PSTs with similar chemical structures were comparable, but varied significantly between subclasses, with M-toxins showing the lowest sensitivity. For example, STX showed a greater than 50-fold higher RMR than M4 and M6 by LC-HRMS. The MS instrument, scan mode and polarity also had significant impacts on RMRs and should be carefully considered when semiquantitating PSTs by LC-MS. As a demonstration of their utility, the RMRs determined were applied to the semiquantitation of PSTs in contaminated mussels, showing good agreement with results from calibration with CRMs.

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LeBlanc, Patricia, Nadine Merkley, Krista Thomas, Nancy I. Lewis, Khalida Békri, Susan LeBlanc Renaud, Frances R. Pick, Pearse McCarron, Christopher O. Miles, and Michael A. Quilliam. "Isolation and Characterization of [D-Leu1]microcystin-LY from Microcystis aeruginosa CPCC-464." Toxins 12, no. 2 (January 23, 2020): 77. http://dx.doi.org/10.3390/toxins12020077.

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[D-Leu1]MC-LY (1) ([M + H]+ m/z 1044.5673, Δ 2.0 ppm), a new microcystin, was isolated from Microcystis aeruginosa strain CPCC-464. The compound was characterized by 1H and 13C NMR spectroscopy, liquid chromatography–high resolution tandem mass spectrometry (LC–HRMS/MS) and UV spectroscopy. A calibration reference material was produced after quantitation by 1H NMR spectroscopy and LC with chemiluminescence nitrogen detection. The potency of 1 in a protein phosphatase 2A inhibition assay was essentially the same as for MC-LR (2). Related microcystins, [D-Leu1]MC-LR (3) ([M + H]+ m/z 1037.6041, Δ 1.0 ppm), [D-Leu1]MC-M(O)R (6) ([M + H]+ m/z 1071.5565, Δ 2.0 ppm) and [D-Leu1]MC-MR (7) ([M + H]+ m/z 1055.5617, Δ 2.2 ppm), were also identified in culture extracts, along with traces of [D-Leu1]MC-M(O2)R (8) ([M + H]+ m/z 1087.5510, Δ 1.6 ppm), by a combination of chemical derivatization and LC–HRMS/MS experiments. The relative abundances of 1, 3, 6, 7 and 8 in a freshly extracted culture in the positive ionization mode LC–HRMS were ca. 84, 100, 3.0, 11 and 0.05, respectively. These and other results indicate that [D-Leu1]-containing MCs may be more common in cyanobacterial blooms than is generally appreciated but are easily overlooked with standard targeted LC–MS/MS screening methods.

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Lefebvre, Donatien, Kevin Blanco-Valle, Jacques-Antoine Hennekinne, Stéphanie Simon, François Fenaille, François Becher, and Yacine Nia. "Multiplex Detection of 24 Staphylococcal Enterotoxins in Culture Supernatant Using Liquid Chromatography Coupled to High-Resolution Mass Spectrometry." Toxins 14, no. 4 (March 31, 2022): 249. http://dx.doi.org/10.3390/toxins14040249.

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Staphylococcal food poisoning outbreaks are caused by the ingestion of food contaminated with staphylococcal enterotoxins (SEs). Among the 27 SEs described in the literature to date, only a few can be detected using immuno-enzymatic-based methods that are strongly dependent on the availability of antibodies. Liquid chromatography, coupled to high-resolution mass spectrometry (LC-HRMS), has, therefore, been put forward as a relevant complementary method, but only for the detection of a limited number of enterotoxins. In this work, LC-HRMS was developed for the detection and quantification of 24 SEs. A database of 93 specific signature peptides and LC-HRMS parameters was optimized using sequences from 24 SEs, including their 162 variants. A label-free quantification protocol was established to overcome the absence of calibration standards. The LC-HRMS method showed high performance in terms of specificity, sensitivity, and accuracy when applied to 49 enterotoxin-producing strains. SE concentrations measured depended on both SE type and the coagulase-positive staphylococci (CPS) strain. This study indicates that LC-MS is a relevant alternative and complementary tool to ELISA methods. The advantages of LC-MS clearly lie in both the multiplex analysis of a large number of SEs, and the automated analysis of a high number of samples.

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Lucci, Paolo, Javier Saurina, and Oscar Núñez. "Trends in LC-MS and LC-HRMS analysis and characterization of polyphenols in food." TrAC Trends in Analytical Chemistry 88 (March 2017): 1–24. http://dx.doi.org/10.1016/j.trac.2016.12.006.

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Marchand, Jérémy, Yann Guitton, Estelle Martineau, Anne-Lise Royer, David Balgoma, Bruno Le Bizec, Patrick Giraudeau, and Gaud Dervilly. "Extending the Lipidome Coverage by Combining Different Mass Spectrometric Platforms: An Innovative Strategy to Answer Chemical Food Safety Issues." Foods 10, no. 6 (May 28, 2021): 1218. http://dx.doi.org/10.3390/foods10061218.

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From a general public health perspective, a strategy combining non-targeted and targeted lipidomics MS-based approaches is proposed to identify disrupted patterns in serum lipidome upon growth promoter treatment in pigs. Evaluating the relative contributions of the platforms involved, the study aims at investigating the potential of innovative analytical approaches to highlight potential chemical food safety threats. Serum samples collected during an animal experiment involving control and treated pigs, whose food had been supplemented with ractopamine, were extracted and characterised using three MS strategies: Non-targeted RP LC-HRMS; the targeted Lipidyzer™ platform (differential ion mobility associated with shotgun lipidomics) and a homemade LC-HRMS triglyceride platform. The strategy enabled highlighting specific lipid profile patterns involving various lipid classes, mainly in relation to cholesterol esters, sphingomyelins, lactosylceramide, phosphatidylcholines and triglycerides. Thanks to the combination of non-targeted and targeted MS approaches, various compartments of the pig serum lipidome could be explored, including commonly characterised lipids (Lipidyzer™), triglyceride isomers (Triglyceride platform) and unique lipid features (non-targeted LC-HRMS). Thanks to their respective characteristics, the complementarity of the three tools could be demonstrated for public health purposes, with enhanced coverage, level of characterization and applicability.

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Raml, Reingard, Maria Ratzer, Barbara Obermayer-Pietsch, Anton Mautner, Thomas R. Pieber, Frank M. Sinner, and Christoph Magnes. "Quantifying vitamin D and its metabolites by LC/Orbitrap MS." Analytical Methods 7, no. 20 (2015): 8961–66. http://dx.doi.org/10.1039/c5ay01583a.

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We developed a HPLC-HRMS method for the determination of 25(OH)D₂, 25(OH)D₃, epi-25(OH)D₃, and vitamins D₂and D₃as well as 24,25(OH)₂D₃.

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Ameline, Alice, Laurie Gheddar, Jean-Sébastien Raul, and Pascal Kintz. "Characterization of letrozole in human hair using LC-MS/MS and confirmation by LC-HRMS: Application to a doping case." Journal of Chromatography B 1162 (January 2021): 122495. http://dx.doi.org/10.1016/j.jchromb.2020.122495.

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Estevez, Pablo, David Castro, José Manuel Leão-Martins, Manoëlla Sibat, Angels Tudó, Robert Dickey, Jorge Diogene, Philipp Hess, and Ana Gago-Martinez. "Toxicity Screening of a Gambierdiscus australes Strain from the Western Mediterranean Sea and Identification of a Novel Maitotoxin Analogue." Marine Drugs 19, no. 8 (August 15, 2021): 460. http://dx.doi.org/10.3390/md19080460.

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Dinoflagellate species of the genera Gambierdiscus and Fukuyoa are known to produce ciguatera poisoning-associated toxic compounds, such as ciguatoxins, or other toxins, such as maitotoxins. However, many species and strains remain poorly characterized in areas where they were recently identified, such as the western Mediterranean Sea. In previous studies carried out by our research group, a G. australes strain from the Balearic Islands (Mediterranean Sea) presenting MTX-like activity was characterized by LC-MS/MS and LC-HRMS detecting 44-methyl gambierone and gambieric acids C and D. However, MTX1, which is typically found in some G. australes strains from the Pacific Ocean, was not detected. Therefore, this study focuses on the identification of the compound responsible for the MTX-like toxicity in this strain. The G. australes strain was characterized not only using LC-MS instruments but also N2a-guided HPLC fractionation. Following this approach, several toxic compounds were identified in three fractions by LC-MS/MS and HRMS. A novel MTX analogue, named MTX5, was identified in the most toxic fraction, and 44-methyl gambierone and gambieric acids C and D contributed to the toxicity observed in other fractions of this strain. Thus, G. australes from the Mediterranean Sea produces MTX5 instead of MTX1 in contrast to some strains of the same species from the Pacific Ocean. No CTX precursors were detected, reinforcing the complexity of the identification of CTXs precursors in these regions.

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Maldini, Mariateresa, Gilda D’Urso, Giordana Pagliuca, Giacomo Luigi Petretto, Marzia Foddai, Francesca Romana Gallo, Giuseppina Multari, Donatella Caruso, Paola Montoro, and Giorgio Pintore. "HPTLC-PCA Complementary to HRMS-PCA in the Case Study of Arbutus unedo Antioxidant Phenolic Profiling." Foods 8, no. 8 (July 27, 2019): 294. http://dx.doi.org/10.3390/foods8080294.

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A comparison between High-Performance Thin-Layer Chromatography (HPTLC) analysis and Liquid Chromatography High Resolution Mass Spectrometry (LC–HRMS), coupled with Principal Component Analysis (PCA) was carried out by performing a combined metabolomics study to discriminate Arbutus unedo (A. unedo) plants. For a rapid digital record of A. unedo extracts (leaves, yellow fruit, and red fruit collected in La Maddalena and Sassari, Sardinia), HPTLC was used. Data were then analysed by PCA with the results of the ability of this technique to discriminate samples. Similarly, extracts were acquired by non-targeted LC–HRMS followed by unsupervised PCA, and then by LC–HRMS (MS) to identify secondary metabolites involved in the differentiation of the samples. As a result, we demonstrated that HPTLC may be applied as a simple and reliable untargeted approach to rapidly discriminate extracts based on tissues and/or geographical origins, while LC–HRMS could be used to identify which metabolites are able to discriminate samples.

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Beck, Olof, and Magnus Ericsson. "Methods for urine drug testing using one-step dilution and direct injection in combination with LC–MS/MS and LC–HRMS." Bioanalysis 6, no. 17 (August 2014): 2229–44. http://dx.doi.org/10.4155/bio.14.192.

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Qu, Lihua, Wenjun Wang, Debin Zeng, Yaxin Lu, and Zheng Yin. "Quantitative performance of online SPE-LC coupled to Q-Exactive for the analysis of sofosbuvir in human plasma." RSC Advances 5, no. 119 (2015): 98269–77. http://dx.doi.org/10.1039/c5ra20233g.

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Hemmer, Selina, Sascha K. Manier, Svenja Fischmann, Folker Westphal, Lea Wagmann, and Markus R. Meyer. "Comparison of Three Untargeted Data Processing Workflows for Evaluating LC-HRMS Metabolomics Data." Metabolites 10, no. 9 (September 21, 2020): 378. http://dx.doi.org/10.3390/metabo10090378.

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The evaluation of liquid chromatography high-resolution mass spectrometry (LC-HRMS) raw data is a crucial step in untargeted metabolomics studies to minimize false positive findings. A variety of commercial or open source software solutions are available for such data processing. This study aims to compare three different data processing workflows (Compound Discoverer 3.1, XCMS Online combined with MetaboAnalyst 4.0, and a manually programmed tool using R) to investigate LC-HRMS data of an untargeted metabolomics study. Simple but highly standardized datasets for evaluation were prepared by incubating pHLM (pooled human liver microsomes) with the synthetic cannabinoid A-CHMINACA. LC-HRMS analysis was performed using normal- and reversed-phase chromatography followed by full scan MS in positive and negative mode. MS/MS spectra of significant features were subsequently recorded in a separate run. The outcome of each workflow was evaluated by its number of significant features, peak shape quality, and the results of the multivariate statistics. Compound Discoverer as an all-in-one solution is characterized by its ease of use and seems, therefore, suitable for simple and small metabolomic studies. The two open source solutions allowed extensive customization but particularly, in the case of R, made advanced programming skills necessary. Nevertheless, both provided high flexibility and may be suitable for more complex studies and questions.

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Lin, Xiao, Ling Chai, Hong Rui Zhu, Yongjun Zhou, Yaoyao Shen, Kai Hao Chen, Fan Sun, Bu Ming Liu, Shi Hai Xu, and Hou Wen Lin. "Applying molecular networking for targeted isolation of depsipeptides." RSC Advances 11, no. 5 (2021): 2774–82. http://dx.doi.org/10.1039/d0ra09388b.

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Birbeck, Johnna A., Nicholas J. Peraino, Grace M. O’Neill, Julia Coady, and Judy A. Westrick. "Dhb Microcystins Discovered in USA Using an Online Concentration LC–MS/MS Platform." Toxins 11, no. 11 (November 10, 2019): 653. http://dx.doi.org/10.3390/toxins11110653.

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Based on current structural and statistical calculations, thousands of microcystins (MCs) can exist; yet, to date, only 246 MCs were identified and only 12 commercial MC standards are available. Standard mass spectrometry workflows for known and unknown MCs need to be developed and validated for basic and applied harmful algal bloom research to advance. Our investigation focuses on samples taken in the spring of 2018 from an impoundment fed by Oser and Bischoff Reservoirs, Indiana, United States of America (USA). The dominant cyanobacterium found during sampling was Planktothrix agardhii. The goal of our study was to identify and quantify the MCs in the impoundment sample using chemical derivatization and mass spectrometry. Modifying these techniques to use online concentration liquid chromatography tandem mass spectrometry (LC–MS/MS), two untargeted MCs have been identified, [d-Asp3, Dhb7]-MC-LR and [Dhb7]-MC-YR. [Dhb7]-MC-YR is not yet reported in the literature to date, and this was the first reported incidence of Dhb MCs in the United States. Furthermore, it was discovered that the commercially available [d-Asp3]-MC-RR standard was [d-Asp3, Dhb7]-MC-RR. This study highlights a workflow utilizing online concentration LC–MS/MS, high-resolution MS (HRMS), and chemical derivatization to identify isobaric MCs.

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Sasse, Michael, and Matthias Rainer. "Mass Spectrometric Methods for Non-Targeted Screening of Metabolites: A Future Perspective for the Identification of Unknown Compounds in Plant Extracts." Separations 9, no. 12 (December 7, 2022): 415. http://dx.doi.org/10.3390/separations9120415.

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Phyto products are widely used in natural products, such as medicines, cosmetics or as so-called “superfoods”. However, the exact metabolite composition of these products is still unknown, due to the time-consuming process of metabolite identification. Non-target screening by LC-HRMS/MS could be a technique to overcome these problems with its capacity to identify compounds based on their retention time, accurate mass and fragmentation pattern. In particular, the use of computational tools, such as deconvolution algorithms, retention time prediction, in silico fragmentation and sophisticated search algorithms, for comparison of spectra similarity with mass spectral databases facilitate researchers to conduct a more exhaustive profiling of metabolic contents. This review aims to provide an overview of various techniques and tools for non-target screening of phyto samples using LC-HRMS/MS.

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You, Youwen, Rachel M. Proctor, Kevin Guo, Xiaoqing Li, Evan Xue, Fuyu Guan, and Mary A. Robinson. "Use of high resolution/accurate mass full scan/data-dependent acquisition for targeted/non-targeted screening in equine doping control." Analytical Methods 13, no. 13 (2021): 1565–75. http://dx.doi.org/10.1039/d0ay02297g.

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A targeted/non-targeted LC-HRMS/MS method for equine doping screening analysis was developed using a QE-Plus Orbitrap mass spectrometer combined with an in-house built compound database and spectral library.

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Theofel, Nadine, Marlene Wagner, Elke Vejmelka, Stefan Scholtis, and Michael Tsokos. "Herbal Medicine Must Be Treated with Care—A Case Report on Aconitine." Forensic Sciences 1, no. 1 (May 5, 2021): 25–32. http://dx.doi.org/10.3390/forensicsci1010005.

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Pathologists usually only request a screening for natural toxic substances if plant material has been observed during autopsy or if there exists a hint in the police investigation file. This situation is aggravated by the fact that most toxins are not covered by typical immunoassays and gas chromatography–mass spectrometry (GC–MS) profiling systems. In addition, only a few forensic toxicological libraries based on liquid chromatography coupled to high-resolution tandem mass spectrometry (LC–HRMS/MS) exist. In the following case, femoral blood and urine were applied to systematic toxicological analysis (STA). However, the concentrations determined in blood did not lead to death. Consequently, a liquid chromatography high-resolution tandem mass spectrometry (LC–HRMS/MS) screening approach was applied. Aconitine was quantitated in all specimens taken during autopsy and urine and bile fluid screened for aconitine metabolites. Aconitine, jesaconitine, hypaconitine, and mesaconitine were found in the root piece collected from the duodenum. Apart from aconitine, no other alkaloids were detected in the urine or in the femoral blood sample. The highest concentrations of aconitine were found in gastric content (55.2 μg/mL), bile fluid (11.7 μg/mL), and liver (9.14 μg/g), and least in femoral blood (0.15 μg/mL) and cerebrospinal fluid (0.07 μg/mL). The liver/peripheral blood ratio amounted to 61 L/kg and indicated that aconitine undergoes postmortem redistribution. During our metabolism investigation, we found 3-dehydrogen-aconitine in the urine and bile fluid sample and N-deethyl-aconitine only in the bile fluid sample. If the routine GC–MS screening approach does not come up with a toxin, then LC–HRMS/MS profiling could represent the method of choice. In this case aconitine was identified. The concentrations determined were compared to those reported in literature and clearly indicate that the deceased died due to an aconitine overdose.

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Lima, Gesiane S., Nerilson M. Lima, Jussara V. Roque, Deborah V. A. de Aguiar, João V. A. Oliveira, Gabriel F. dos Santos, Andrea R. Chaves, and Boniek G. Vaz. "LC-HRMS/MS-Based Metabolomics Approaches Applied to the Detection of Antifungal Compounds and a Metabolic Dynamic Assessment of Orchidaceae." Molecules 27, no. 22 (November 16, 2022): 7937. http://dx.doi.org/10.3390/molecules27227937.

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The liquid chromatography–mass spectrometry (LC-MS)-based metabolomics approach is a powerful technology for discovering novel biologically active molecules. In this study, we investigated the metabolic profiling of Orchidaceae species using LC-HRMS/MS data combined with chemometric methods and dereplication tools to discover antifungal compounds. We analyze twenty ethanolic plant extracts from Vanda and Cattleya (Orchidaceae) genera. Molecular networking and chemometric methods were used to discriminate ions that differentiate healthy and fungal-infected plant samples. Fifty-three metabolites were rapidly annotated through spectral library matching and in silico fragmentation tools. The metabolomic profiling showed a large production of polyphenols, including flavonoids, phenolic acids, chromones, stilbenoids, and tannins, which varied in relative abundance across species. Considering the presence and abundance of metabolites in both groups of samples, we can infer that these constituents are associated with biochemical responses to microbial attacks. In addition, we evaluated the metabolic dynamic through the synthesis of stilbenoids in fungal-infected plants. The tricin derivative flavonoid- and the loliolide terpenoidfound only in healthy plant samples, are promising antifungal metabolites. LC-HRMS/MS, combined with state-of-the-art tools, proved to be a rapid and reliable technique for fingerprinting medicinal plants and discovering new hits and leads.

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Abbas, Ioana M., Marija Vranic, Holger Hoffmann, Ahmed H. El-Khatib, María Montes-Bayón, Heiko M. Möller, and Michael G. Weller. "Investigations of the Copper Peptide Hepcidin-25 by LC-MS/MS and NMR." International Journal of Molecular Sciences 19, no. 8 (August 2, 2018): 2271. http://dx.doi.org/10.3390/ijms19082271.

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Hepcidin-25 was identified as the main iron regulator in the human body, and it by binds to the sole iron-exporter ferroportin. Studies showed that the N-terminus of hepcidin is responsible for this interaction, the same N-terminus that encompasses a small copper(II)-binding site known as the ATCUN (amino-terminal Cu(II)- and Ni(II)-binding) motif. Interestingly, this copper-binding property is largely ignored in most papers dealing with hepcidin-25. In this context, detailed investigations of the complex formed between hepcidin-25 and copper could reveal insight into its biological role. The present work focuses on metal-bound hepcidin-25 that can be considered the biologically active form. The first part is devoted to the reversed-phase chromatographic separation of copper-bound and copper-free hepcidin-25 achieved by applying basic mobile phases containing 0.1% ammonia. Further, mass spectrometry (tandem mass spectrometry (MS/MS), high-resolution mass spectrometry (HRMS)) and nuclear magnetic resonance (NMR) spectroscopy were employed to characterize the copper-peptide. Lastly, a three-dimensional (3D) model of hepcidin-25 with bound copper(II) is presented. The identification of metal complexes and potential isoforms and isomers, from which the latter usually are left undetected by mass spectrometry, led to the conclusion that complementary analytical methods are needed to characterize a peptide calibrant or reference material comprehensively. Quantitative nuclear magnetic resonance (qNMR), inductively-coupled plasma mass spectrometry (ICP-MS), ion-mobility spectrometry (IMS) and chiral amino acid analysis (AAA) should be considered among others.

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Koelmel, Jeremy P., Xiangdong Li, Sarah M. Stow, Mark J. Sartain, Adithya Murali, Robin Kemperman, Hiroshi Tsugawa, et al. "Lipid Annotator: Towards Accurate Annotation in Non-Targeted Liquid Chromatography High-Resolution Tandem Mass Spectrometry (LC-HRMS/MS) Lipidomics Using a Rapid and User-Friendly Software." Metabolites 10, no. 3 (March 12, 2020): 101. http://dx.doi.org/10.3390/metabo10030101.

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Lipidomics has great promise in various applications; however, a major bottleneck in lipidomics is the accurate and comprehensive annotation of high-resolution tandem mass spectral data. While the number of available lipidomics software has drastically increased over the past five years, the reduction of false positives and the realization of obtaining structurally accurate annotations remains a significant challenge. We introduce Lipid Annotator, which is a user-friendly software for lipidomic analysis of data collected by liquid chromatography high-resolution tandem mass spectrometry (LC-HRMS/MS). We validate annotation accuracy against lipid standards and other lipidomics software. Lipid Annotator was integrated into a workflow applying an iterative exclusion MS/MS acquisition strategy to National Institute of Standards and Technology (NIST) SRM 1950 Metabolites in Frozen Human Plasma using reverse phase LC-HRMS/MS. Lipid Annotator, LipidMatch, and MS-DIAL produced consensus annotations at the level of lipid class for 98% and 96% of features detected in positive and negative mode, respectively. Lipid Annotator provides percentages of fatty acyl constituent species and employs scoring algorithms based on probability theory, which is less subjective than the tolerance and weighted match scores commonly used by available software. Lipid Annotator enables analysis of large sample cohorts and improves data-processing throughput as compared to previous lipidomics software.

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Ferraris, Quintin, Armando Alcazar, and Michael C. Qian. "Profiling polar lipids in whey protein phospholipid concentrate by LC-HRMS/MS." Food Chemistry 374 (April 2022): 131495. http://dx.doi.org/10.1016/j.foodchem.2021.131495.

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Silva, Ana Carolina R., Carol Cristine da Silva, Rafael Garrett, and Claudia M. Rezende. "Comprehensive lipid analysis of green Arabica coffee beans by LC-HRMS/MS." Food Research International 137 (November 2020): 109727. http://dx.doi.org/10.1016/j.foodres.2020.109727.

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Kasiotis, Konstantinos M., Eirini Baira, Electra Manea-Karga, Dimitra Nikolopoulou, Konstantinos Ganas, and Kyriaki Machera. "Investigating a human pesticide intoxication incident: The importance of robust analytical approaches." Open Chemistry 19, no. 1 (January 1, 2021): 107–18. http://dx.doi.org/10.1515/chem-2021-0193.

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Abstract A human intoxication incident attributed to pesticide abuse was investigated using cutting-edge analytical methodologies. An LC-ESI-MS/MS method, based on a hybrid solid-phase extraction protocol (hybrid-SPE), was applied for the detection and quantification of several pesticides and metabolites in human biological fluids. Concomitantly, an UHPLC-HRMS method was applied to investigate potential metabolites, assisted by a complementary GC-MS method to elucidate the presence of plausible pesticides co-formulants. The LC-ESI-MS/MS method exhibited acceptable mean recoveries at the lower limit of quantification (LLOQ) and three additional levels, varying from 85 to 106% for all analytes and matrices. In serum, urine, and gastric fluid samples, the suspect compounds, namely chlorpyrifos and myclobutanil, predominated. Gastric fluid samples contained the highest concentrations of chlorpyrifos (39,800 ng/mL) and myclobutanil (18,800 ng/mL), while the neonicotinoid imidacloprid was also quantified, below 30 ng/mL. Notwithstanding, the UHPLC-HRMS analysis unveiled several metabolites of chlorpyrifos and myclobutanil. In parallel, GC-MS analysis, corroborated the presence of several co-formulants in gastric fluid samples, exemplified by m- and o-xylene, and cyclohexanone. Overall, three analytical methods were implemented to elucidate the chemical causality of a human intoxication incident. The presence of suspected active substances, one additional, and several metabolites and co-formulants were documented.

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Estevez, Pablo, Manoella Sibat, José Manuel Leão-Martins, Pedro Reis Costa, Ana Gago-Martínez, and Philipp Hess. "Liquid Chromatography Coupled to High-Resolution Mass Spectrometry for the Confirmation of Caribbean Ciguatoxin-1 as the Main Toxin Responsible for Ciguatera Poisoning Caused by Fish from European Atlantic Coasts." Toxins 12, no. 4 (April 21, 2020): 267. http://dx.doi.org/10.3390/toxins12040267.

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Ciguatera poisoning (CP) is a common seafood intoxication mainly caused by the consumption of fish contaminated by ciguatoxins. Recent studies showed that Caribbean ciguatoxin-1 (C-CTX1) is the main toxin causing CP through fish caught in the Northeast Atlantic, e.g., Canary Islands (Spain) and Madeira (Portugal). The use of liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) combined with neuroblastoma cell assay (N2a) allowed the initial confirmation of the presence of C-CTX1 in contaminated fish samples from the abovementioned areas, nevertheless the lack of commercially available reference materials for these particular ciguatoxin (CTX) analogues has been a major limitation to progress research. The EuroCigua project allowed the preparation of C-CTX1 laboratory reference material (LRM) from fish species (Seriola fasciata) from the Madeira archipelago (Portugal). This reference material was used to implement a liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS) for the detection of C-CTX1, acquisition of full-scan as well as collision-induced mass spectra of this particular analogue. Fragmentation pathways were proposed based on fragments obtained. The optimized LC-HRMS method was then applied to confirm C-CTX1 in fish (Bodianus scrofa) caught in the Selvagens Islands (Portugal).

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Lima, Nerilson M., Gesiane S. Lima, Gabriel F. dos Santos, Gagan Preet, Lanaia I. L. Maciel, Teresinha de Jesus A. S. Andrade, Marcel Jaspars, Andrea R. Chaves, and Boniek G. Vaz. "Assessing the Effectiveness of Chemical Marker Extraction from Amazonian Plant Cupuassu (Theobroma grandiflorum) by PSI-HRMS/MS and LC-HRMS/MS." Metabolites 13, no. 3 (March 1, 2023): 367. http://dx.doi.org/10.3390/metabo13030367.

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Employing a combination of liquid chromatography electrospray ionization and paper spray ionization high-resolution tandem mass spectrometry, extracts from cupuassu (Theobroma grandiflorum) pulp prepared with either water, methanol, acetonitrile or combinations thereof were subjected to metabolite fingerprinting. Among the tested extractors, 100% methanol extracted preferentially phenols and cinnamic acids derivatives, whereas acetonitrile and acetonitrile/methanol were more effective in extracting terpenoids and flavonoids, respectively. And while liquid chromatography- mass spectrometry detected twice as many metabolites as paper spray ionization tandem mass spectrometry, the latter proved its potential as a screening technique. Comprehensive structural annotation showed a high production of terpenes, mainly oleanane triterpene derivatives. of the mass spectra Further, five major metabolites with known antioxidant activity, namely catechin, citric acid, epigallocatechin-3′-glucuronide, 5,7,8-trihydroxyflavanone, and asiatic acid, were subjected to molecular docking analysis using the antioxidative enzyme peroxiredoxin 5 (PRDX5) as a model receptor. Based on its excellent docking score, a pharmacophore model of 5,7,8-trihydroxyflavanone was generated, which may help the design of new antioxidants.

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Dwi Widayati, Rieska, Tanti Tanti, Erlana Nindya Maulida, and Martin Luther Silubun. "Identification of Synthetic Cannabinoid 5F-ADB (5F-MDMB-PINACA) and Its Metabolite in Urine Sample Using Liquid Chromatography – High Resolution Mass Spectrometer (LC-HRMS)." Journal of Pure and Applied Chemistry Research 9, no. 2 (August 31, 2020): 91–97. http://dx.doi.org/10.21776/ub.jpacr.2020.009.02.537.

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Synthetic cannabinoids are commonly known as Gorillas Tobacco, Hanomans Tobacco or Ganeshas Tobacco in Indonesia. Those products are camouflaged as a tobacco related to the number of smokers in Indonesia. The 5F-ADB (5F-MDMB-PINACA) has become an issue since 2016. It was undetectable by conventional drug testing methodology such as immunoassay method. GC-MS as a routine method analysis is not recommended also for detecting the metabolites from biological specimen with low concentration. The paper report LC-HRMS based method for identification of 5F-ADB and its metabolites in urine sample. Various of volume injections (1, 3, and 6 µL) was studied. Sample was acidified with concentrate of HCl, then undergo extraction with EXtrelut® Column NT3 prior to LC-HRMS analysis. The full method was operated for MS/dd-MS2 identification. The 5F-ADB and its ester hydrolysis metabolite, 5F-ADB metabolite 7 (C19H27FN3O3+) was detected in urine sample.

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Pelletier, Romain, Thomas Gicquel, Mélanie Simoes Eugenio, Pierre-Jean Ferron, Isabelle Morel, Claire Delehouzé, Marie-Thérèse Dimanche-Boitrel, Morgane Rousselot, and Brendan Le Daré. "A Transversal Approach Combining In Silico, In Vitro and In Vivo Models to Describe the Metabolism of the Receptor Interacting Protein 1 Kinase Inhibitor Sibiriline." Pharmaceutics 14, no. 12 (November 30, 2022): 2665. http://dx.doi.org/10.3390/pharmaceutics14122665.

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Sibiriline is a novel drug inhibiting receptor-interacting protein 1 kinase (RIPK1) and necroptosis, a regulated form of cell death involved in several disease models. In this study, we aimed to investigate the metabolic fate of sibiriline in a cross-sectional manner using an in silico prediction, coupled with in vitro and in vivo experiments. In silico predictions were performed using GLORYx and Biotransformer 3.0 freeware; in vitro incubation was performed on differentiated human HepaRG cells, and in vivo experiments including a pharmacokinetic study were performed on mice treated with sibiriline. HepaRG culture supernatants and mice plasma samples were analyzed with ultra-high-performance liquid chromatography, coupled with tandem mass spectrometry (LC-HRMS/MS). The molecular networking bioinformatics tool applied to LC-HRMS/MS data allowed us to visualize the sibiriline metabolism kinetics. Overall, 14 metabolites, mostly produced by Phase II transformations (glucuronidation and sulfation) were identified. These data provide initial reassurance regarding the toxicology of this new RIPK1 inhibitor, although further studies are required.

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Slobodchikova, Irina, Reajean Sivakumar, Md Samiur Rahman, and Dajana Vuckovic. "Characterization of Phase I and Glucuronide Phase II Metabolites of 17 Mycotoxins Using Liquid Chromatography—High-Resolution Mass Spectrometry." Toxins 11, no. 8 (July 24, 2019): 433. http://dx.doi.org/10.3390/toxins11080433.

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Routine mycotoxin biomonitoring methods do not include many mycotoxin phase I and phase II metabolites, which may significantly underestimate mycotoxin exposure especially for heavily metabolized mycotoxins. Additional research efforts are also needed to measure metabolites in vivo after exposure and to establish which mycotoxin metabolites should be prioritized for the inclusion during large-scale biomonitoring efforts. The objective of this study was to perform human in vitro microsomal incubations of 17 mycotoxins and systematically characterize all resulting metabolites using liquid chromatography–high-resolution mass spectrometry (LC-HRMS). The results obtained were then used to build a comprehensive LC-MS library and expand a validated 17-mycotoxin method for exposure monitoring to screening of additional 188 metabolites, including 100 metabolites reported for the first time. The final method represents one of the most comprehensive LC-HRMS methods for mycotoxin biomonitoring or metabolism/fate studies.

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Kioussi, Maroula K., Emmanouil M. Lyris, Yiannis S. Angelis, Maria Tsivou, Michael A. Koupparis, and Costas G. Georgakopoulos. "A generic screening methodology for horse doping control by LC–TOF-MS, GC–HRMS and GC–MS." Journal of Chromatography B 941 (December 2013): 69–80. http://dx.doi.org/10.1016/j.jchromb.2013.10.008.

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Gampfer, Tanja M., Lea Wagmann, Matthias J. Richter, Svenja Fischmann, Folker Westphal, and Markus R. Meyer. "Toxicokinetic Studies and Analytical Toxicology of the New Synthetic Opioids Cyclopentanoyl-Fentanyl and Tetrahydrofuranoyl-Fentanyl." Journal of Analytical Toxicology 44, no. 5 (February 4, 2020): 449–60. http://dx.doi.org/10.1093/jat/bkaa010.

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Abstract The growing number of new synthetic opioids (NSO) on the new psychoactive substances (NPS) market bears new challenges in toxicology. As their toxicodynamics and particularly their toxicokinetics are usually unknown, impact on human health is not yet fully understood. Detection of the 2 NSO cyclopentanoyl-fentanyl (CP-F) and tetrahydrofuranoyl-fentanyl (THF-F) was first reported in 2016. Both were involved in several fatal intoxication cases, but no detailed information about their toxicological characteristics is available so far. The main purpose of this study was therefore to investigate the in vitro toxicokinetics and in vivo analytical toxicology of CP-F and THF-F by means of liquid chromatography high-resolution tandem mass spectrometry (LC-HRMS/MS). These studies included metabolic stability, phase I and II metabolism, isozyme mapping, plasma protein binding and detectability in LC-HRMS/MS standard urine screening approaches (SUSA) using rat urine samples. In total, 12 phase I metabolites of CP-F and 13 of THF-F were identified, among them 9 metabolites described for the first time. Overall, N-dealkylations, hydroxylations and dihydroxylations were the main metabolic reactions. The cytochrome P450 (CYP) isozymes mainly involved were CYP2D6 and CYP3A4, leading to elevated drug levels and intoxications in CYP2D6 poor metabolizers. CP-F showed a high plasma protein binding of 99%, which may increase the risk of toxicity by simultaneous intake of other highly bound drugs. Detectability studies showed that neither the parent compounds nor their metabolites were detectable in rat urine using LC-HRMS/MS SUSA. However, a more sophisticated analytical strategy was successfully applied and should be used for analytical confirmation of an intake of CP-F and/or THF-F.

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Simões-Pires, Cláudia A., Fabianne M. Farias, Andrew Marston, Emerson F. Queiroz, Célia G. Chaves, Amélia T. Henriques, and Kurt Hostettmann. "Indole Monoterpenes with Antichemotactic Activity from Psychotria myriantha: Chemotaxonomic Significance." Natural Product Communications 1, no. 12 (December 2006): 1934578X0600101. http://dx.doi.org/10.1177/1934578x0600101206.

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The alkaloid extract of the aerial parts of Psychotria myriantha (Rubiaceae) displayed antichemotactic activity on polymorphonuclear leukocytes (PMN) assessed by the Boyden chamber assay. On analysis of the crude extract by LC/APCI/MS and LC/UV/DAD, two major constituents could be detected. In order to rapidly identify the active compounds, a microfractionation was conducted during LC/UV/DAD analysis. By this means, both the collected compounds could be assayed separately in the Boyden chamber and were shown to inhibit PMN chemotaxis. Their isolation was performed by semi-preparative HPLC and their structures elucidated by classical spectroscopic methods, including UV, NMR, MS and HRMS. Both compounds showed characteristics of monoterpene indole glucoside alkaloids; one of them was identified as strictosidinic acid and the other was a new natural product, myrianthosine. The antichemotactic activity of the compounds may be related to an antiacute inflammation activity.

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Oberacher, Herbert, Vera Reinstadler, Marco Kreidl, Michael Stravs, Juliane Hollender, and Emma Schymanski. "Annotating Nontargeted LC-HRMS/MS Data with Two Complementary Tandem Mass Spectral Libraries." Metabolites 9, no. 1 (December 23, 2018): 3. http://dx.doi.org/10.3390/metabo9010003.

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Tandem mass spectral databases are indispensable for fast and reliable compound identification in nontargeted analysis with liquid chromatography–high resolution tandem mass spectrometry (LC-HRMS/MS), which is applied to a wide range of scientific fields. While many articles now review and compare spectral libraries, in this manuscript we investigate two high-quality and specialized collections from our respective institutes, recorded on different instruments (quadrupole time-of-flight or QqTOF vs. Orbitrap). The optimal range of collision energies for spectral comparison was evaluated using 233 overlapping compounds between the two libraries, revealing that spectra in the range of CE 20–50 eV on the QqTOF and 30–60 nominal collision energy units on the Orbitrap provided optimal matching results for these libraries. Applications to complex samples from the respective institutes revealed that the libraries, combined with a simple data mining approach to retrieve all spectra with precursor and fragment information, could confirm many validated target identifications and yield several new Level 2a (spectral match) identifications. While the results presented are not surprising in many ways, this article adds new results to the debate on the comparability of Orbitrap and QqTOF data and the application of spectral libraries to yield rapid and high-confidence tentative identifications in complex human and environmental samples.

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Mairinger, Teresa, Martin Loos, and Juliane Hollender. "Characterization of water-soluble synthetic polymeric substances in wastewater using LC-HRMS/MS." Water Research 190 (February 2021): 116745. http://dx.doi.org/10.1016/j.watres.2020.116745.

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Ding, Chi, Li Pang, Zhao-Xun Liang, Kau Goh, Evgenia Glukhov, William Gerwick, and Lik Tan. "MS/MS-Based Molecular Networking Approach for the Detection of Aplysiatoxin-Related Compounds in Environmental Marine Cyanobacteria." Marine Drugs 16, no. 12 (December 13, 2018): 505. http://dx.doi.org/10.3390/md16120505.

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Certain strains of cyanobacteria produce a wide array of cyanotoxins, such as microcystins, lyngbyatoxins and aplysiatoxins, that are associated with public health issues. In this pilot study, an approach combining LC-MS/MS and molecular networking was employed as a rapid analytical method to detect aplysiatoxins present in four environmental marine cyanobacterial samples collected from intertidal areas in Singapore. Based on 16S-ITS rRNA gene sequences, these filamentous cyanobacterial samples collected from Pulau Hantu were determined as Trichodesmium erythraeum, Oscillatoria sp. PAB-2 and Okeania sp. PNG05-4. Organic extracts were prepared and analyzed on LC-HRMS/MS and Global Natural Product Social Molecular Networking (GNPS) for the presence of aplysiatoxin-related molecules. From the molecular networking, six known compounds, debromoaplysiatoxin (1), anhydrodebromoaplysiatoxin (2), 3-methoxydebromoaplysiatoxin (3), aplysiatoxin (4), oscillatoxin A (5) and 31-noroscillatoxin B (6), as well as potential new analogues, were detected in these samples. In addition, differences and similarities in molecular networking clusters related to the aplysiatoxin molecular family were observed in extracts of Trichodesmium erythraeum collected from two different locations and from different cyanobacterial species found at Pulau Hantu, respectively.

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Lima, Raissa, Marcos Vinicius T. Silva, Brendo A. Gomes, Ellis Helena B. C. Macedo, Michele N. Santana, Ana Claudia F. Amaral, Jefferson R. A. Silva, et al. "Chemical Profile and Hematoprotective Activity of Artisanal Jabuticaba (Plinia jabuticaba) Wine and Derived Extracts." Fermentation 9, no. 2 (February 6, 2023): 157. http://dx.doi.org/10.3390/fermentation9020157.

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The alcoholic fermentation of jabuticaba berries (Plinia spp.) originates from a beverage with an intense taste and aroma, popularly known as jabuticaba wine (JW). In addition, polyphenols transferred from fruit peels to the final product turn this beverage into a promising source of bioactive agents. Here, the chemical profile and antioxidant potential of artisanal JW and derivative extracts were determined. Volatile organic compounds were determined by HS-SPME/GC-MS analysis. The wine was dried by lyophilization and subjected to liquid-liquid partitioning (water: ethyl acetate), resulting in three fractions (JWF1-3). ABTS•+ and DPPH•+ scavenging assays were performed to evaluate the antioxidant capacity. In addition, the extracts’ hematoprotective activity was evaluated against oxidative stress. Finally, the extracts were analyzed by LC-HRMS/MS. HS-SPME/GC-MS analysis highlighted 1,8-cineole as the main compound that contributes to the camphor/mint flavor. JWF2 and JWF3 displayed the highest antioxidant capacity. JWF2 stood out for preventing oxidative damage in red blood cells at 7.8 µg·mL−1 The maximal protection of ascorbic acid occurred at 8.8 µg·mL−1. The LC-HRMS/MS analysis allowed the annotation of seventeen compounds, most of them with recognized antioxidant activity such as anthocyanins, catechins, flavanols, and phenolic acids. The results presented herein reinforce JW as a pleasant beverage with bioactive potential.

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Reveglia, Pierluigi, Maria Luisa Raimondo, Marco Masi, Alessio Cimmino, Genoveffa Nuzzo, Gaetano Corso, Angelo Fontana, Antonia Carlucci, and Antonio Evidente. "Untargeted and Targeted LC-MS/MS Based Metabolomics Study on In Vitro Culture of Phaeoacremonium Species." Journal of Fungi 8, no. 1 (January 6, 2022): 55. http://dx.doi.org/10.3390/jof8010055.

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Grapevine (Vitis vinifera L.) can be affected by many different biotic agents, including tracheomycotic fungi such as Phaeomoniella chlamydospora and Phaeoacremonium minimum, which are the main causal agent of Esca and Petri diseases. Both fungi produce phytotoxic naphthalenone polyketides, namely scytalone and isosclerone, that are related to symptom development. The main objective of this study was to investigate the secondary metabolites produced by three Phaeoacremonium species and to assess their phytotoxicity by in vitro bioassay. To this aim, untargeted and targeted LC-MS/MS-based metabolomics were performed. High resolution mass spectrometer UHPLC-Orbitrap was used for the untargeted profiling and dereplication of secondary metabolites. A sensitive multi reaction monitoring (MRM) method for the absolute quantification of scytalone and isosclerone was developed on a UPLC-QTrap. Different isolates of P. italicum, P. alvesii and P. rubrigenum were grown in vitro and the culture filtrates and organic extracts were assayed for phytotoxicity. The toxic effects varied within and among fungal isolates. Isosclerone and scytalone were dereplicated by matching retention times and HRMS and MS/MS data with pure standards. The amount of scytalone and isosclerone differed within and among fungal species. To our best knowledge, this is the first study that applies an approach of LC-MS/MS-based metabolomics to investigate differences in the metabolic composition of organic extracts of Phaeoacremonium species culture filtrates.

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Monga, Gaganpreet Kaur, Anima Ghosal, and Dil Ramanathan. "To Develop the Method for UHPLC-HRMS to Determine the Antibacterial Potential of a Central American Medicinal Plant." Separations 6, no. 3 (July 29, 2019): 37. http://dx.doi.org/10.3390/separations6030037.

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The development of antibiotic resistance by microbials has long been acknowledged. The major challenge worldwide is to develop novel, natural, and potent antibiotics against the multidrug resistant bacteria. In this study, our aim was to develop the method for a highly sensitive instrument, ultra-high performance liquid chromatograph-high resolution mass spectrometer (UHPLC-HRMS), to evaluate the antibacterial property of a natural product. Aechmea magdalenae (Andre) Andre ex Baker, a plant belonging to the family Bromeliaceae, a native of Central America was used in this study. Based on the available literature, it was hypothesized that Aechmea magdalenae has antibacterial activity. In addition, the profiling done on A. magdalenae using gas chromatography-mass spectrometry (GC-MS) also revealed the presence of medicinally important chemical compounds, such as acetic acid. Minimum inhibitory concentration (MIC) of dried Aechmea plant extract was determined for the first time using 96-well plate assay, followed by determination of antibacterial potential using LC-MS. The reason being that other dried methanolic plant extracts, such as Vismia macrophylla, lined up for antibacterial testing have dark extracts, for which determining the antibacterial potential and reading the results with the naked eye would be challenging. To overcome the situation of dark plant extracts, a generalized novel LC-MS method was developed that was used for the plant A. magdalenae, and would be used further for other plants. A blue indicator called resazurin was added to the wells; resazurin, upon incubation with the living cells, got reduced to resorufin (which was pink), while it remained blue with bacterial growth inhibition. The mass difference created due to reduction of resazurin to resorufin was detected by using LTQ Orbitrap Discovery in positive ion mode to determine the antibacterial activity of the plant extract. The sample preparation for LC-MS assay included centrifugation of the samples taken from 96-well plate, followed by filtration of the supernatant, before exposing them to C-18 column. The results obtained from full scan LC-MS spectrum consistently demonstrated the presence of resorufin from wells with bacterial growth, and resazurin from wells with inhibition through peaks of relevant masses.

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Shi, Wen, Xiang Yuan, Kuiqing Cui, Hui Li, Penghui Fu, Saif-Ur Rehman, Deshun Shi, Qingyou Liu, and Zhipeng Li. "LC-MS/MS Based Metabolomics Reveal Candidate Biomarkers and Metabolic Changes in Different Buffalo Species." Animals 11, no. 2 (February 20, 2021): 560. http://dx.doi.org/10.3390/ani11020560.

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Consumers have shown more and more interest in high-quality and healthy dairy products and buffalo milk is commercially more viable than other milks in producing superior dairy products due to its higher contents of fat, crude protein, and total solids. Metabolomics is one of the most powerful strategies in molecular mechanism research however, little study has been focused on the milk metabolites in different buffalo species. Therefore, the aim of this study was to explore the underlying molecular mechanism of the fatty synthesis and candidate biomarkers by analyzing the metabolomic profiles. Milk of three groups of buffaloes, including 10 Mediterranean, 12 Murrah, and 10 crossbred buffaloes (Murrah × local swamp buffalo), were collected and UPLC-Q-Orbitrap HRMS was used to obtain the metabolomic profiles. Results showed that milk fatty acid in Mediterranean buffalo was significantly higher than Murrah buffalo and crossbred buffalo. A total of 1837/726 metabolites was identified in both positive and negative electrospray ionization (ESI±) mode, including 19 significantly different metabolites between Mediterranean and Murrah buffalo, and 18 different metabolites between Mediterranean and crossbred buffalo. We found 11 of the different metabolites were both significantly different between Mediterranean vs. Murrah group and Mediterranean vs crossbred group, indicating that they can be used as candidate biomarkers of Mediterranean buffalo milk. Further analysis found that the different metabolites were mainly enriched in fat synthesis related pathways such as fatty acid biosynthesis, unsaturated fatty acid biosynthesis, and linoleic acid metabolism, indicating that the priority of different pathways affected the milk fat content in different buffalo species. These specific metabolites may be used as biomarkers in the identification of milk quality and molecular breeding of high milk fat buffalo.

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Devreux, Vincent, Sylvain Combet, Emmanuelle Clabaux, and Estelle D. Gueneau. "From pigments to coloured napkins: comparative analyses of primary aromatic amines in cold water extracts of printed tissues by LC-HRMS and LC-MS/MS." Food Additives & Contaminants: Part A 37, no. 11 (September 22, 2020): 1985–2010. http://dx.doi.org/10.1080/19440049.2020.1802068.

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Feith, André, Attila Teleki, Michaela Graf, Lorenzo Favilli, and Ralf Takors. "HILIC-Enabled 13C Metabolomics Strategies: Comparing Quantitative Precision and Spectral Accuracy of QTOF High- and QQQ Low-Resolution Mass Spectrometry." Metabolites 9, no. 4 (April 2, 2019): 63. http://dx.doi.org/10.3390/metabo9040063.

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Dynamic 13C-tracer-based flux analyses of in vivo reaction networks still require a continuous development of advanced quantification methods applying state-of-the-art mass spectrometry platforms. Utilizing alkaline HILIC chromatography, we adapt strategies for a systematic quantification study in non- and 13C-labeled multicomponent endogenous Corynebacterium glutamicum extracts by LC-QTOF high resolution (HRMS) and LC-QQQ tandem mass spectrometry (MS/MS). Without prior derivatization, a representative cross-section of 17 central carbon and anabolic key intermediates were analyzed with high selectivity and sensitivity under optimized ESI-MS settings. In column detection limits for the absolute quantification range were between 6.8–304.7 (QQQ) and 28.7–881.5 fmol (QTOF) with comparable linearities (3–5 orders of magnitude) and enhanced precision using QQQ-MRM detection. Tailor-made preparations of uniformly (U)13C-labeled cultivation extracts for isotope dilution mass spectrometry enabled the accurate quantification in complex sample matrices and extended linearities without effect on method parameters. Furthermore, evaluation of metabolite-specific m+1-to-m+0 ratios (ISR1:0) in non-labeled extracts exhibited sufficient methodical spectral accuracies with mean deviations of 3.89 ± 3.54% (QTOF) and 4.01 ± 3.01% (QQQ). Based on the excellent HILIC performance, conformity analysis of time-resolved isotopic enrichments in 13C-tracer experiments revealed sufficient spectral accuracy for QQQ-SIM detection. However, only QTOF-HRMS ensures determination of the full isotopologue space in complex matrices without mass interferences.

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Yu, Huilan, Shilei Liu, Daoming Sun, Chengxin Pei, and Yu Xiang. "Identification of N-Methyl Bis(2-(Alkyloxy-Alkylphosphoryloxy)Ethyl) Amines by LC-HRMS/MS." American Journal of Analytical Chemistry 05, no. 13 (2014): 820–27. http://dx.doi.org/10.4236/ajac.2014.513091.

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Xynos, Nikos, Aikaterini Termentzi, Nikolas Fokialakis, Leandros A. Skaltsounis, and Nektarios Aligiannis. "Supercritical CO2 extraction of mastic gum and chemical characterization of bioactive fractions using LC-HRMS/MS and GC–MS." Journal of Supercritical Fluids 133 (March 2018): 349–56. http://dx.doi.org/10.1016/j.supflu.2017.10.011.

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Tanna, Sangeeta, John Ogwu, and Graham Lawson. "Hyphenated mass spectrometry techniques for assessing medication adherence: advantages, challenges, clinical applications and future perspectives." Clinical Chemistry and Laboratory Medicine (CCLM) 58, no. 5 (April 28, 2020): 643–63. http://dx.doi.org/10.1515/cclm-2019-0820.

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Abstract:

AbstractNonadherence to prescribed pharmacotherapy is an understated public health problem globally and is costing many patients their chance to return to good health and healthcare systems billions. Clinicians need an accurate assessment of adherence to medications to aid the clinical decision-making process in the event of poor patient progress and to maximise the patient health outcomes from the drug therapies prescribed. An overview of indirect and direct methods used to measure medication adherence is presented, highlighting the potential for accurate measuring of drugs in biological samples using hyphenated mass spectrometry (MS) techniques to provide healthcare professionals with a reliable evidence base for clinical decision making. In this review we summarise published applications of hyphenated MS techniques for a diverse range of clinical areas demonstrating the rise in the use of such direct methods for assessing medication adherence. Although liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods using plasma, serum and urine samples are the most popular, in recent years increased attention has been given to liquid chromatography high-resolution mass spectrometry (LC-HRMS) methods and alternative biosample matrices including hair, saliva and blood microsamples. The advantages and challenges of using hyphenated MS techniques to address this healthcare problem are also discussed alongside future perspectives.

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Journal articles on the topic 'LC-MS/MS and LC/HRMS'

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