4.4 Article

Improved separation of fentanyl isomers using metal cation adducts and high-resolution ion mobility-mass spectrometry

Journal

DRUG TESTING AND ANALYSIS
Volume -, Issue -, Pages -

Publisher

WILEY
DOI: 10.1002/dta.3550

Keywords

fentanyl; ion mobility-mass spectrometry (IM-MS); isomers

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Fentanyl, a potent opioid, has raised concerns due to its illegal production and distribution, leading to misuse, overdose, and deaths. This study aimed to develop a rapid method for detecting and separating fentanyl isomers using ion mobility-mass spectrometry (IM-MS). Several strategies for improved differentiation were implemented, resulting in confident detection and subsequent quantitative analysis.
Fentanyl is a potent synthetic opioid that has attracted significant attention due to its illegal production and distribution, resulting in misuse, overdose, and fatalities. Because numerous fentanyl analogs, including structural isomers, with different potency have been discovered in the field, there is a critical need to continue developing analytical methodologies capable of accurate identification in forensic and clinical laboratories. This study aimed to develop a rapid method for detecting and separating fentanyl isomers based on ion mobility-mass spectrometry (IM-MS), where IM separates gas-phase ions based on differences in their size, shape, and charge. Several strategies for improved differentiation were implemented, including using unconventional cation adducts (e.g., alkali and transition metals) and data post-processing by high-resolution demultiplexing. A collection of collision cross section (CCS) values for the various metal ion adducts was gathered, which can be used to improve confidence of identification in future samples. Notable examples, such as [M + Cu](+) and [M + Ag](+) adducts, contributed to significant improvement of resolution between isomers. Furthermore, the addition of high-resolution post-processing provided resolving power of >150, which constitutes a significant increase in comparison with the normal 50-60 obtained with low-resolution drift tube instruments. Collectively, these improved separation strategies allowed for confident detection and subsequent quantitative analysis. The optimized IM-MS method resulted in quantification of fentanyl in human urine with limits of detection and quantification of 13 pg/mL and 40 pg/mL, respectively.

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