CERTIFICAÇÃO DE MATERIAL DE REFERÊNCIA INTERNO PARA CANABINOIDE SINTÉTICO E SUA APLICAÇÃO NO DESENVOLVIMENTO DE METODOLOGIA ANALÍTICA POR GC-MS

Abstract

Synthetic cannabinoids (SC) are an extensive family of New Psychoactive Substances (NPS) that have been widely available on the market of drug abuse since 2004. These have effects similar to those presented by Δ9-THC, but may have potentiated psychoactive effects (up to 100 times more intense) due to their greater affinity for the receptors of the cannabinoid system, causing various health problems for the user and may even lead to death, thus being a public health problem worldwide. Combating both NPS and SC is a major challenge due to the variety of structures and their rapid modification in order to circumvent current legislation. Certified Reference Materials (CRM) for these substances are important and essential in the control of drug abuse, whether in qualitative or quantitative analyses. However, the high price and bureaucracy involved in acquiring them, as they are controlled substances, makes it difficult or even impossible to conduct relevant research on these substances. Therefore, the present work aimed to develop a proposal for a certification protocol for an “internal” RM seized by the Civil Police of the state of Mato Grosso do Sul (PC-MS). Using ABNT ISO 17034, GUIDEs 35 and 31 as a base, the aim was to develop an analytical methodology using Gas Chromatography (GC), interfaced with Mass Spectrometry (MS), for use by the security forces of the state of Mato Grosso do Sul in the control of this class of substances. The blotters containing the unknown substance were characterized using FTIR and GC–MS, DIMS being identified as ADB-Butinaca (N-[(1S)-1-(aminocarbonyl)-2,2-dimethylpropyl]-1 -1H-indazole-3-carboxamide), an NPS of the SC class. This was extracted from a mass of 12.1697g of seized material with HPLC grade methanol, under sonification for 10 minutes. The extract was filtered, evaporated, dried in an oven for 48 hours, obtaining 758mg of recovered substance, indicating a concentration of 6.23% m/m or 62.29mg/g of blotters. The degree of purity of the substance was determined by Differential Scanning Calorimetry (DSC) and Quantitative Nuclear Magnetic Resonance (qNMR), these being 98.93% (± 0.23) and 97.24 (± 1.46), respectively, with an average purity of 98.09% (± 0.96) of the CRM candidate. Considering the determined purity degree, an analytical curve was then constructed with concentrations ranging from 1.5 to 10mg L-1, applying the MDMA-SILD-DIAZ-LSD.M program by PC-MS, obtaining a linearity coefficient (R) of 0.9996. The stability of the CRM candidate was rated from day 1, 90 and 180 after its isolation, obtaining degrees of purity of 99.05 (± 0.33), 98.81 (± 0.09) and 98.33 % (± 0.21), respectively, representing a purity decay of 0.72 % in the sample of the CRM candidate.