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Lysergic acid diethylamide (LSD) analogs, often referred to as new psychoactive substances, are synthesized to mimic controlled substances while evading drug regulations. This study emphasizes the challenges of identifying these compounds, particularly their isomeric forms. Gas chromatography–mass spectrometry (GC–MS) and UV spectroscopy were employed to analyze 13 LSD analogs. The effects of different solvents on the detection of these analogs were analyzed, demonstrating that solvents like diethyl ether, tert-butyl methyl ether, dichloromethane and acetone provided the best sensitivity and stability. Methanol, on the other hand, causes alcoholysis of many LSD analogs, which may lead to false results. Additionally, effective chromatographic separation of isomers was established, including LSD, MiPLA, LAMPA, 1P-LSD and 1P-MiPLA, as well as 1cP-LSD and 1cP-MiPLA, which is crucial for accurate identification. The elution order of the determined compounds with the use of developed chromatographic method was as follows: LSD, MiPLA, LAMPA, AL-LAD, LSZ, 2-Br-LSD, ALD-52, 1P-LSD, 1P-MiPLA, 1B-LSD, 1V-LSD, 1cP-LSD and 1cP-MiPLA. Differences in ion ratios observed in mass spectrometry (MS) were also analyzed to distinguish between closely related compounds. Several key ions for LSD analogs were able to be identified, including 221, 208, 207, 196, 194, 192, 181, 167, 154, 152 and 128 m/z. In analogs with an N-diethyl group (or variants like N-methyl-propyl in LAMPA or N-methyl-isopropyl in MiPLA), mass spectra showed fragments 100, 72 and 58 m/z. For LSZ, the cyclic group at R1 produces ions 98 and 70 m/z. Analogs with an N6 allyl group (e.g., AL-LAD) show a characteristic ion 247 m/z. This method allows for the correct differentiation of structural isomers based on their unique ion fragmentation patterns and relative intensities. UV spectroscopy was used as a supplementary tool for screening, though it has limitations in analyzing complex mixtures. This work contributes to the forensic identification of designer LSD analogs, ensuring reliable detection for legal and toxicological investigations. Full article

The rapid dispersion of new psychoactive substances (NPS) presents challenges to customs services and analytical laboratories, which are involved in their detection and characterization. When the seized material is limited in quantity or of a complex nature, or when the target substance is present in very small amounts, the need to use advanced analytical techniques, efficient workflows and chemo-informatics tools is essential for the complete identification and elucidation of these substances. The current work describes the application of such a workflow in the analysis of a single blotter paper, seized by Swedish customs, that led to the identification of a lysergic acid diethylamide (LSD) derivative, 1-butyl-lysergic acid diethylamide (1B-LSD). Such blotter paper generally contains an amount in the range of 30–100 ug. This substance, which is closely related to 1-propionyl-lysergic acid diethylamide (1P-LSD), seems to have only recently reached the drug street market. Its identification was made possible by comprehensively combining gas chromatography with mass spectrometry detection (GC–MS), liquid chromatography coupled with high-resolution tandem MS (LC–HR-MS/MS), Orbitrap-MS and both 1D and 2D nuclear-magnetic-resonance (NMR) spectroscopy. All the obtained data have been managed, assessed, processed and evaluated using a chemo-informatics platform to produce the effective chemical and structural identification of 1B-LSD in the seized material. Full article