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Developing a qNMR method for purity profiling of crack-cocaine sa | 52622
Journal of Clinical Toxicology

Journal of Clinical Toxicology
Open Access

ISSN: 2161-0495

Developing a qNMR method for purity profiling of crack-cocaine samples seized by police forces in northeastern Brazil


4th Global Summit on Toxicology

August 24-26, 2015 Philadelphia, USA

Eduardo de Jesus Oliveira1 and Rony Anderson Rezende Costa2

Posters-Accepted Abstracts: J Clin Toxicol

Abstract :

Illicit use of Crack-cocaine has become a major health issue in Brazil which is currently a large consumer of world's cocaine according
to UN statistics. The present work describes the development of a 1H-qNMR method to assay crack cocaine samples seized by
police forces in northeastern Brazil. Samples were weighted and dissolved in D2O acidified with DCl. The internal standard used was
the sodium salt of 3-(trimethylsilyl)-2, 2, 3, 3,-D-4 propionic acid (TSP-D4). The same samples assayed with the 1H-qNMR method
were submitted to analysis by a validated quantification method based on reversed-phase high performance liquid chromatography
with diode array detection for comparison of the cocaine content. Also, a GC/MS method was used for confirmation of the impurities
detected with the NMR method. The results revealed that the average content of cocaine in the samples was above 70% (w/w). There
was a large variability in the purity of samples as determined by both methods (5.2-89.1%, w/w for 1H-qNMR and from 4.9 to
93.8% w/w for the HPLC method). The best correlation between the HPLC and the 1H-qNMR values was obtained when using the
integration values of the 3.6 ppm singlet signal corresponding to methyl ester protons (r2=0.83). The main impurity detected in the
1H-NMR spectra of the samples was phenacetin, which was found in 84% of the samples. This adulterant was confirmed by GC/MS
analysis. The developed 1H-qNMR can be regarded as a simple, convenient and fast screening method to assist in the purity profiling
of crack cocaine samples.

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