325. The application of 19F NMR spectroscopy for the analysis of fluorinated new psychoactive substances (NPS)

Cui-mei Liu, Chun-hui Song, Wei Jia, Zhen-dong Hua and Qi Liao; Forensic Science International; (2022); DOI: 10.1016/j.forsciint.2022.111450

In this study, fluorine-19 nuclear magnetic resonance spectroscopy (19F NMR) served as a highly specific tool for identification of fluorinated new psychoactive substances (NPS) as well as a suitable analytical method for the accurate quantification of fluorinated NPS in different seized samples. In the first part of the study, 19F NMR spectroscopy of a number of different fluorinated NPS, including 51 synthetic cannabinoids, 8 synthetic cathinones, 7 phenethylamines, 8 fentanyl analogues, and 9 other types of compounds was conducted. The chemical shifts and multiplet of the primary fluorides (RCH2F), fluorobenzenes (ortho-ArF, meta-ArF, and para-ArF), and trifluoromethylbenzenes (ArCF3) were discussed in detail to illustrate the role of 19F signals as special fingerprints in assisting the structure identification of fluorine-containing NPS. To the best of our knowledge, this study is the largest evaluation of fluorinated NPS compounds by 19F NMR. The second part of this study dealt with the problems encountered in the 19F quantification procedure and the criteria to be considered for successful quantification by 19F NMR. General high field (HF)- and low field (LF)- 19F qNMR methods for the quantification of fluorinated NPS were established after the thorough discussion of NMR spectrum acquisition and processing parameters such as: transmitter frequency offset (O1P), spin-lattice relaxation time (T1), and different baseline correction methods. The limit of quantifications (LOQs) for HF-19F qNMR varied between 0.1 mg/mL and 0.2 mg/mL, and for LF-19F qNMR varied between 1.0 mg/mL and 2.0 mg/mL. The limit of detections (LODs) for HF-19F qNMR varied between 0.03 mg/mL and 0.06 mg/mL, and for LF-19F qNMR varied between 0.3 mg/mL and 0.6 mg/mL. Finally, the developed methods were applied for the quantification of fluorinated-NPS in seventeen herbal blends, e-liquid, tablet, and powder NPS seizures.