The quantification of minor alkaloids in seized cocaine can provide information for drug profiling and law enforcement initiatives. This work presents the development and validation of an analytical method to quantitate minor alkaloids in cocaine samples using gas chromatography with flame ionization detector, after derivatization. The method was validated in accordance with the ISO/IEC 17.025:2017 requirements. The calibration was linear (determination coefficient (R2) ≥ 0.998), ranging from 1.0 to 3,500 mg L-1 for all target analytes with suitable selectivity and precision (relative standard deviation lower than 10%). The method showed stability and robustness with respect to analytical parameter variations and presented good accuracy (recovery ranging from 90 to 108%). The method was considered adequate to routine forensic analysis in simultaneous quantification of anhydroecgonine methyl ester, anhydroecgonine, methylecgonine, tropacocaine, norcocaine, N-formylcocaine, trimethoxycocaine, ecgonine, benzoylecgonine, trans- and cis-cinnamoylcocaine. Eleven cocaine samples seized in different Brazilian regions were analyzed and their relative amounts of tropacocaine and trimethoxycocaine with respect to cocaine indicate both the possible varieties of coca leaf used for cocaine production and the likely origin of drug samples (Bolivia/Peru or Colombia). The contents of other minor alkaloids depict aspects of sample history such as purification by oxidation, hydrolysis and dehydration by thermal processes.

This work describes results of chemical profiling by gas chromatography with flame ionization detector (GC-FID) of the main components (purity, oxidation level, and cutting agents) in 642 street cocaine samples seized in five different Brazilian States between 2011 and 2014. The analysis revealed the presence of cocaine with mean content of 49.8%. Freebase samples showed cocaine average content of 66.0%, whereas hydrochloride and not determined (n.d.) present cocaine content of 44.5% and 11.8%, respectively. Cocaine base samples show moderately (16%) to not oxidized (81%) levels, whereas cocaine hydrochloride samples exhibit moderate (37%) to high (22%) oxidation degrees. Approximately 34% of all the analyzed samples did not have any adulterant identified. Base cocaine samples are even less adulterated (42% uncut) with phenacetin being present in 53% (average content of 15%). Caffeine and lidocaine were mostly found in hydrochloride samples, while the n.d. samples show a combination of either phenacetin or a caffeine/lidocaine mixture. A mass balance approach is presented and seizures information can be combined to deliver intelligence and statistical analysis that might contribute to the understanding of street cocaine composition scenario. A total of 269 samples were characterized as crack cocaine showing phenacetin as the main adulterant and presenting an average cocaine content of 68.3%.

From a set of 159 samples seized by Brazilian Federal Police between 2010 to 2013 in the Federal District, the major component chemical profiling routine analyses revealed the presence of cocaine with purity range of 5.5 to 99.9% (mean 69.8%). Most cocaine base samples show moderately and not oxidized levels, whereas cocaine hydrochloride samples exhibit moderate to high oxidation degrees. More than 40% of the analyzed samples did not have any adulterant. Phenacetin was the most abundant adulterant (24% average purity). Aminopyrine, a new adulterant, was identified and quantified only in cocaine base samples, mainly as a trace adulterant but also as a major compound. In most samples adulterated with aminopyrine, phenacetin was also identified as a major adulterant, suggesting a possible association of the two pharmaceuticals in the cutting process. Aminopyrine was not detected in 2010 seizures, but became a common adulterant throughout the years of 2011 to 2013. A mass balance approach analysis also established that adulterants are responsible for only 12% of the mass of all seizures (i.e., 84 kg), whereas 77% (i.e., 553 kg) is due to alkaloids (cocaine and cis/trans-cinnamoylcocaine), contributing to provide forensic intelligence information to police investigators.

Perfis químicos de cocaína podem fornecer informações relevantes para autoridades da área de segurança pública. Desde 2006, a Polícia Federal tem trabalhado em seu próprio perfil químico de impurezas da cocaína (projeto PeQui). No esforço de estabelecer rotinas de perfil químico, este trabalho descreve os resultados obtidos para identificação de componentes majoritários (pureza da cocaína, grau de oxidação e fármacos utilizados como adulterantes), através da análise por cromatografia gasosa com detector de ionização de chama (GC-FID) de 210 amostras apreendidas em diferentes estados brasileiros entre 2009 e 2012. A pureza média observada para cocaína foi de 71% (expressa como base) e o grau de oxidação, determinado pela medida relativa entre cis/trans-cinamoilcocaína e cocaína, mostrou-se dependente do local de apreensão. A maioria das amostras não oxidadas foram apreendidas nos estados que fazem fronteira com os países produtores. A forma de base livre é a mais comumente encontrada (59%) e mais de 50% das amostras analisadas não apresentaram nenhum adulterante majoritário. Dentre os fármacos adulterantes identificados, fenacetina foi o mais abundante (30% das amostras). Levamisol, cafeína e lidocaína também foram identificados. O projeto PeQui tem sido utilizado regularmente para prover informações técnicas cientificamente embasadas para a análise de inteligência em segurança pública e de dados estatísticos que podem contribuir para um melhor entendimento do tráfico de cocaína.

Cocaine chemical profiling can provide relevant information for law enforcement authorities. Since 2006, Brazilian Federal Police has been working on its own cocaine impurity profiling program (PeQui project). In the effort to establish chemical profiling routines, this work describes major component results (cocaine purity, degree of oxidation and pharmaceutical products used as cutting agents), identified by gas chromatography with flame ionization detection (GC-FID) analysis of 210 samples seized in several Brazilian states between 2009 and 2012. The mean purity of cocaine was 71% (expressed as base) and the degree of oxidation, determined by the relative content between cis/trans-cinnamoylcocaine and cocaine, depends on the location where the seizures were performed. Most of the not oxidized samples were seized on traditional cocaine producer country border states. Cocaine is mainly present in free base form (59%) and more than 50% of the analyzed samples did not have any major adulterant. Among the identified cutting agents, phenacetin was the most abundant (30% of the total samples). Levamisole, caffeine and lidocaine were also identified. The PeQui project has been used on regular basis to provide technical and scientifically based information to law enforcement intelligence analysis and statistical data that might contribute to the better understanding of the cocaine trafficking.