High-resolution accurate mass spectrometry as a technique for characterization of complex lysimeter leachate samples

2016 ◽  
Vol 35 (6) ◽  
pp. 1401-1412 ◽  
Author(s):  
Laurence H. Hand ◽  
Samantha J. Marshall ◽  
Mansoor Saeed ◽  
Mark Earll ◽  
Stephen T. Hadfield ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Accurate Mass ◽  
Accurate Mass Spectrometry ◽  
High Resolution Accurate Mass

scholarly journals Screening and Characterization of Reactive Compounds with In Vitro Peptide-Trapping and Liquid Chromatography/High-Resolution Accurate Mass Spectrometry

2013 ◽  
Vol 19 (2) ◽  
pp. 297-307 ◽  
Author(s):  
Cong Wei ◽  
Louis S. Chupak ◽  
Thomas Philip ◽  
Benjamin M. Johnson ◽  
Robert Gentles ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Resolution ◽  
High Throughput Screening ◽  
Accurate Mass ◽  
Full Scan ◽  
Accurate Mass Spectrometry ◽  
High Resolution Accurate Mass

The present study describes a novel methodology for the detection of reactive compounds using in vitro peptide-trapping and liquid chromatography–high-resolution accurate mass spectrometry (LC-HRMS). Compounds that contain electrophilic groups can covalently bind to nucleophilic moieties in proteins and form adducts. Such adducts are thought to be associated with drug-mediated toxicity and therefore represent potential liabilities in drug discovery programs. In addition, reactive compounds identified in biological screening can be associated with data that can be misinterpreted if the reactive nature of the compound is not appreciated. In this work, to facilitate the triage of hits from high-throughput screening (HTS), a novel assay was developed to monitor the formation of covalent peptide adducts by compounds suspected to be chemically reactive. The assay consists of in vitro incubations of test compounds (under conditions of physiological pH) with synthetically prepared peptides presenting a variety of nucleophilic moieties such as cysteine, lysine, histidine, arginine, serine, and tyrosine. Reaction mixtures were analyzed using full-scan LC-HRMS, the data were interrogated using postacquisition data mining, and modified amino acids were identified by subsequent LC-HRMS/mass spectrometry. The study demonstrated that in vitro nucleophilic peptide trapping followed by LC-HRMS analysis is a useful approach for screening of intrinsically reactive compounds identified from HTS exercises, which are then removed from follow-up processes, thus obviating the generation of data from biochemical activity assays.

scholarly journals In-Depth Glycoproteomic Characterization of γ-Conglutin by High-Resolution Accurate Mass Spectrometry

PLoS ONE ◽  
2013 ◽  
Vol 8 (9) ◽  
pp. e73906 ◽  
Author(s):  
Silvia Schiarea ◽  
Lolita Arnoldi ◽  
Roberto Fanelli ◽  
Eric De Combarieu ◽  
Chiara Chiabrando
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Accurate Mass ◽  
Accurate Mass Spectrometry ◽  
High Resolution Accurate Mass

scholarly journals Non-targeted Screening of Commercial CBD Products in the United States Reveals Common Contamination and Adulteration

2020 ◽  
Author(s):  
Ben Orsburn
Keyword(s):  
United States ◽  
Mass Spectrometry ◽  
High Resolution ◽  
The United States ◽  
Mass Spectrometry Data ◽  
Accurate Mass ◽  
Targeted Screening ◽  
Accurate Mass Spectrometry ◽  
High Concentrations ◽  
High Resolution Accurate Mass

AbstractThe production of hemp and products derived from these plants that contain zero to trace amounts of the psychoactive cannabinoid tetrahydrocannabidiol (THC) is a rapidly growing new market in the United States. The most common products today contain relatively high concentrations of the compound cannabidiol (CBD). Recent studies have investigated commercial CBD products using targeted assays and have found varying degrees of misrepresentation and contamination of these products. To expand on previous studies, we demonstrate the application of non-targeted screening by high resolution accurate mass spectrometry to more comprehensively identify potential adulterants and contaminants. We find evidence to support previous conclusions that CBD products are commonly misrepresented in terms of cannabinoid concentrations present. Specifically, we observe a wide variation in relative THC concentrations across the product tested, with some products containing 10-fold more relative signal than others. In addition, we find that several products appear to be purposely adulterated with over the counter drugs such as caffeine and melatonin. We also observe multiple small molecule contaminants that are typically linked to improper production or packaging methods in food or pharmaceutical production. Finally, we present high resolution accurate mass spectrometry data and tandem MS/MS fragments supporting the presence of trace amounts of fluorofentanyl in a single mail order CBD product. We conclude that the CBD industry would benefit from more robust testing regulations and that the cannabis testing industry, in general, would benefit from the use of non-targeted screening technologies.

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