Mass spectral similarity mapping applied to fentanyl analogs

Moorthy, Arun S.; Kearsley, Anthony J.; Mallard, W. Gary; Wallace, W.E.

doi:10.1016/j.forc.2020.100237

Cited by 31 publications

(34 citation statements)

References 37 publications

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“…This is an initial facet of identifying an unknown analyte using the instrument's library matching program which can be extremely valuable but need to be considered with caution when assigning a chemical structure to an unknown analyte. [149][150][151] Thus, subsequent analyses involving quadrupole time-of-flight high resolution mass spectrometry (QTOF-MS) couped to an ultra-high performance liquid chromatography (UHPLC) unit, nuclear magnetic resonance (NMR) and infrared spectroscopy (IR) were needed in order to fully identify acrylfentanyl as the opioid. The amount of the acrylfentanyl hydrochloride was eventually determined using high performance liquid chromatography and triple quadrupole spectrometry (LC-MS-MS).…”

Section: Acrylfentanylmentioning

confidence: 99%

Gas Chromatography-Mass Spectrometry Analysis of Synthetic Opioids Belonging to the Fentanyl Class: A Review

Valdez

2021

Critical Reviews in Analytical Chemistry

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The rising number of deaths caused by fentanyl overdosing in the US due to the overwhelming illicit use of this synthetic opioid has started a global campaign to develop efficient ways to control its production and distribution as well as discovering efficient antidotes to mitigate its lethal effects. Another important vein of focused research established by various agencies lies in the development of efficient and practical protocols for the detection of this opioid and analogs thereof in various matrices, whether environmental or biological in nature, particularly in the field of gas chromatography-mass spectrometry (GC-MS). The following review will cover the literature dealing with the detection and identification of synthetic opioids belonging to the fentanyl class by GC-MS means and hyphenated versions of the technique. Detailed descriptions will be given for the GC-MS methods employed for the analysis of the opioid, starting with the nature of the extraction protocol employed prior to analysis to the actual findings presented by the cited reports. Great effort has gone into describing the methods involved in each paper in a detailed manner and these have been compiled by year in tables at the end of each section for the reader's convenience. Lastly, the review will end with concluding remarks about the state of GC-MS analysis with regards to these powerful opioids and what lies ahead for this analytical field.

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Section: Acrylfentanylmentioning

confidence: 99%

Gas Chromatography-Mass Spectrometry Analysis of Synthetic Opioids Belonging to the Fentanyl Class: A Review

Valdez

2021

Critical Reviews in Analytical Chemistry

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“…Examples include Desorption ElectroSpray Ionization (DESI) [28][29][30], Paper-Spray (PS) [31][32][33], Low Temperature Plasma (LTP) ionization [34], Atmospheric Solids Analysis Probe (ASAP) [35] and Direct Analysis in Real Time (DART) [36][37][38][39][40]. When coupled with high-resolution accurate mass spectrometry and MS/MS techniques, the identification and characterization of unexpected or novel drug substances may potentially be achieved using these approaches, via assignment of the molecular formulae of the observed ions and by similarities in MS/MS fragmentation behavior compared to structurally homologous known substances within an established drug class [41][42][43][44].…”

Section: Introductionmentioning

confidence: 99%

Trace Residue Identification, Characterization and Longitudinal Monitoring of the Novel Synthetic Opioid β-U10, from Discarded Drug Paraphernalia

West

Fitzgerald

Hopkins

et al. 2022

Preprint

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Empirical data regarding dynamic alterations in illicit drug supply markets in response to the COVID-19 pandemic, including the potential for introduction of novel drug substances and/or increased poly-drug combinations at the ‘street’ level (i.e., directly proximal to the point of consumption), is currently lacking. Here, a high-throughput strategy employing ambient ionization-mass spectrometry is described for the trace residue identification, characterization and longitudinal monitoring of illicit drug substances found within >6,600 discarded drug paraphernalia (DDP) samples collected during a pilot study of an early warning system for illicit drug use in Melbourne, Australia from August 2020-February 2021, while significant COVID-19 lockdown conditions were imposed. The utility of this approach is demonstrated for the de novo identification and structural characterization of β-U10, a previously unreported naphthamide analogue within the ‘U-series’ of synthetic opioid drugs, including differentiation from its α-U10 isomer without need for sample preparation or chromatographic separation prior to analysis. Notably, β-U10 was observed with 23 other drug substances, most commonly in temporally distinct clusters with heroin, etizolam and diphenhydramine, and in a total of 182 different poly-drug combinations. Finally, longitudinal monitoring of the number and weekly ‘average signal intensity’ (ASI) values of identified substances, developed here as a semi-quantitative proxy indicator of changes in availability, relative purity and compositions of street level drug samples, revealed that increases in the number of identifications and ASI for β-U10 and etizolam coincided with a 50% decrease in the number of positive detections and an order of magnitude decrease in the ASI for heroin.

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“…In terms of novel data analysis and interpretation, Gilbert et al demonstrated how principal component analysis can be used for the classification of fentanyl analogues based on their gas chromatography mass spectrometry (GC-MS) spectra [34]. Moorthy et al showed the ability to use GC-MS data combined with hybrid similarity searching [35] and mass spectral similarity mapping to identify previously unseen analogs [36].…”

Section: Introductionmentioning

confidence: 99%

Development and evaluation of a synthetic opioid targeted gas chromatography mass spectrometry (GC‐MS) method

Sisco

Burns

Moorthy

2021

Journal of Forensic Sciences

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As seized drug casework becomes increasingly complex due to the continued prevalence of emerging drugs, laboratories are often looking for new analytical approaches including developing methods for the analysis of specific compounds classes. Recent efforts have focused on the development of targeted gas chromatography mass spectrometry (GC-MS) confirmation methods to compliment the information-rich screening results produced by techniques like direct analysis in real time mass spectrometry (DART-MS). In this work, a method for the confirmation of synthetic opioids and related compounds was developed and evaluated. An 11-component test solution was used to develop a method that focused on minimizing overlapping retention time acceptance windows and understanding the influence of instrument parameters on reproducibility and sensitivity. Investigated settings included column type, flow rate, temperature program, inlet temperature, source temperature, and tune type. Using a DB-200 column, a 35-min temperature ramped method was created. It was evaluated against a suite of 222 synthetic opioids and related compounds, and successfully differentiated all but four compound pairs based on nonoverlapping retention time acceptance windows or objectively different mass spectra. Compared to a general confirmatory method used in casework, the targeted method was up to 25 times more sensitive and provided at least a two-fold increase in retention time differences.Analysis of extracts from actual case samples successfully demonstrated utility of the method and showed no instance of carryover, although the high polarity column required wider retention time windows than other columns.

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Mass spectral similarity mapping applied to fentanyl analogs

Cited by 31 publications

References 37 publications

Gas Chromatography-Mass Spectrometry Analysis of Synthetic Opioids Belonging to the Fentanyl Class: A Review

Gas Chromatography-Mass Spectrometry Analysis of Synthetic Opioids Belonging to the Fentanyl Class: A Review

Trace Residue Identification, Characterization and Longitudinal Monitoring of the Novel Synthetic Opioid β-U10, from Discarded Drug Paraphernalia

Development and evaluation of a synthetic opioid targeted gas chromatography mass spectrometry (GC‐MS) method

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