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Capillary gas chromatography using a -cyclodextrin forenantiomeric separation of methylamphetamine, its precursors andchloro intermediates after optimization of the derivatization reaction
Abstract
tThe enantiomeric ratio of methylamphetamine (MAMP) is closely related to the optical activity of precur-sors and reagents used for the synthesis and this knowledge can provide useful information concerningthe origins and synthetic methods used for illicit manufacture. The information can be utilized for reg-ulation of the precursors and investigation of the manufacturing sources but this requires analyticalprocedures to determine purity of drug substances, impurity profiling and enantiomeric composition.In this study, a gas chromatography (GC) coupled with mass spectrometry (MS) method using a -cyclodextrin chiral stationary phase was developed and optimized for the simultaneous enantiomericseparations of MAMP and its common precursors, ephedrine, and pseudoephedrine, as well as itschlorointermediates formed during MAMP synthesis by the Emde method, after derivatization with triflu-oroacetic anhydride. The optimization was performed using multivariate statistics (cluster analysis andprincipal components analysis) in order to select and compare optimal experimental conditions. Underthe optimized experimental conditions, the calculated calibration curves showed good linearity range upto 0.1 g/mL for all tested analytes. The limits of detection were in the range of 0.002–0.008 g/mL andthe coefficient of variability was between 1.0 and 3.9%. The method has the advantage of achieving excel-lent precision under repeatability and reproducibility conditions while detection by MS allows for theidentity of analytes to be confirmed in a single analysis. The method was therefore applied satisfactoryto MAMP analysis.
Authors (5)
-
Vasil Simeonov
- University of Sofia Faculty of Chemistry
-
Calum Morrison
- School of Science Faculty of Science and Technology
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- Category:
- Articles
- Type:
- artykuł w czasopiśmie wyróżnionym w JCR
- Published in:
-
JOURNAL OF CHROMATOGRAPHY A
no. 1347,
pages 146 - 156,
ISSN: 0021-9673 - Language:
- English
- Publication year:
- 2014
- Bibliographic description:
- Płotka-Wasylka J., Simeonov V., Morrison C., Biziuk M., Namieśnik J.: Capillary gas chromatography using a -cyclodextrin forenantiomeric separation of methylamphetamine, its precursors andchloro intermediates after optimization of the derivatization reaction// JOURNAL OF CHROMATOGRAPHY A. -Vol. 1347, (2014), s.146-156
- Verified by:
- Gdańsk University of Technology
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