Rapid screening of 2‐benzylbenzimidazole nitazene analogs in suspect counterfeit tablets using Raman, SERS, DART‐TD‐MS, and FT‐IR

Author:

Kimani Martin M.1ORCID,Kern Sara1,Lanzarotta Adam1,Thatcher Michael1,Lorenz Lisa M.1ORCID,Smith Skyler W.1,Collins Melissa1,Howe Gregory W.2,Wetherby Anthony E.3

Affiliation:

1. Office of Regulatory Affairs, Office of Regulatory Science, Forensic Chemistry Center US Food and Drug Administration Cincinnati Ohio USA

2. Office of Regulatory Affairs, Office of Regulatory Science, Pacific Southwest Medical Products Laboratory US Food and Drug Administration Irvine California USA

3. Office of Regulatory Affairs, Office of Regulatory Science, Winchester Engineering Analytical Center US Food and Drug Administration Winchester Massachusetts USA

Abstract

AbstractDeveloping methods to rapidly screen for novel synthetic 2‐benzylbenzimidazole opioids, also known as nitazenes, has become increasingly important due to their high potency. These compounds have potency comparable or exceeding that of fentanyl by up to 10 times and have been implicated in approximately 5% of all drug overdose deaths in the United States in 2021. This paper details the authenticity determination of suspect tablets and the identification of three nitazene analogs (N‐pyrrolidino etonitazene, isotonitazene, and etodesnitazene) in suspect tablets seized at a mail facility using Raman and surface‐enhanced Raman scattering (SERS) with handheld devices, portable Fourier transform infrared spectrometer (FT‐IR), and a direct analysis in real‐time ambient ionization coupled to a thermal desorption unit and a mass spectrometer (DART‐TD‐MS). These methods are rapid and excellent for screening opioids in suspect tablets but could not fully determine the exact structure of some of the nitazene analogs present due to spectral similarities or similar fragmentation patterns. Liquid chromatography–mass spectrometry (LC–MS) confirmed the presence of these nitazene compounds in addition to other opioids/drugs that were in trace quantities. The quantitative high‐performance liquid chromatography coupled with ultraviolet (HPLC‐UV) detection experiments determined that the suspect tablets contained an average of 0.817 mg of N‐pyrrolidino etonitazene per tablet. The results obtained reveal that the simultaneous deployment of these complementary and orthogonal portable analytical techniques as part of a workflow allows suspect tablets to be screened and nitazene‐type drugs to be identified in suspect counterfeit tablets at remote sampling sites.

Publisher

Wiley

Subject

Spectroscopy,Pharmaceutical Science,Environmental Chemistry,Analytical Chemistry

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