High-throughput quantitation of large molecules using multiplexed chromatography and high-resolution/accurate mass LC–MS

Bioanalysis ◽  
2012 ◽  
Vol 4 (9) ◽  
pp. 1013-1024 ◽  
Author(s):  
Keeley Murphy ◽  
Patrick K Bennett ◽  
Nicholas Duczak
Keyword(s):  
High Resolution ◽  
High Throughput ◽  
Accurate Mass ◽  
Large Molecules ◽  
High Resolution Accurate Mass

Analysis of Squalene and Its Transformation By-Products in Latent Fingermarks by Ultrahigh-Pressure Liquid Chromatography-High Resolution Accurate Mass Orbitrap™ Mass Spectrometry

2019 ◽  
Author(s):  
Buddhika Dorakumbura ◽  
Francesco Busetti ◽  
Simon Lewis
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Storage Conditions ◽  
Ultrahigh Pressure ◽  
Accurate Mass ◽  
Rational Approach ◽  
By Products ◽  
Over Time ◽  
High Resolution Accurate Mass

<p>Transformation of squalene and its by-products in fingermarks over time under different storage conditions (light, dark and underwater) was examined through ultrahigh-pressure liquid chromatography high resolution accurate mass Orbitrap™ mass spectrometry. Complications of assessing fingermark compositional variation over time using multiple samples with varying initial compositions were elucidated and a more rational approach was successfully demonstrated. Squalene was detected in all fresh natural fingermarks and the amount ranged between 0.20 to 11.32 μg/5 fingertips. A notable difference in the transformation of squalene was observed with different storage conditions, where a dark aquatic environment accelerated degradation of squalene compared to dark but dry conditions. Squalene monohydroperoxide was extremely short-lived in natural deposits while the amount of squalene epoxide was still increasing relative to the initial amount, after ageing under dark and aquatic conditions for up to 7 days. Some oxidation by-products of cholesterol were also tentatively identified, which exhibited a growth over time against their initial concentration under any of the storage condition tested. These by-products, therefore, show potential as biomarkers for targeted visualisation of aged deposits.</p>

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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