Abstract
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.
Highlights
The Brazilian Federal Police (BFP) has been implementing, since 2006, a chemical profiling program for illicit drugs (PeQui project) designed to provide both accredited forensic reports and scientifically based police intelligence/investigative information.[1]
When the pharmaceutical products typically used to adulterate cocaine were added to the sample, it was noted that only phenacetin and ecgonine-2TMS (TMS: trimethylsilyl derivatized analyte) peaks have resolution below the acceptance criteria (RS = 1.2)
As phenacetin is previously quantified throughout the major component methodology in PeQui program prior minor alkaloid analysis, the integration performance can be evaluated if necessary
Summary
The Brazilian Federal Police (BFP) has been implementing, since 2006, a chemical profiling program for illicit drugs (PeQui project) designed to provide both accredited forensic reports and scientifically based police intelligence/investigative information.[1] The BFP PeQui project mainly deals with samples from international trafficking cocaine seizures, usually involving high amounts (tens to thousands of kg) and high purity (low cut) In this context, the geographic origin of drugs represents one of the most strategic pieces of information for law enforcement agencies.[2]. Ehleringer et al.[8,9] have consistently applied minor alkaloid quantification and isotopic ratio analysis
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