Innovative solutions for enhanced illicit drugs profiling using comprehensive two-dimensional gas chromatography and mass spectrometry technologies

Monograph no. 50

Philip Marriot, Blagoj Mitrevski

Analytical gas chromatographic methods usually rely upon a single dimension (ie single column) high-resolution capillary GC column to provide separation of target analyses. When a matrix is especially complex, the ability of the column to provide adequate resolution is severely compromised. Often, mass spectrometry may provide the ability to uniquely measure the target compounds, but if the matrix generates similar ions to the target compounds, this can lead to confounded analysis. Mass spectrometry offers many potential solutions to the lack of resolution of GC; however, this usually involves selected ion monitoring or similar approaches. This removes the important opportunity to use a full-scan spectrum to match with a database library. In the present project, high-resolution GC analysis using the multidimensional separation method of comprehensive two-dimensional gas chromatography (GCxGC) was used to provide sufficient resolution to allow full-scan acquisition with library confirmation of illicit drug identity. It was shown that the WADA criteria for a selection of test steroid compounds could be suitably met under this new high-resolution environment. In addition, analysis of samples of ecstasy were profiled and all synthetic residues involved in the synthesis of ecstasy could be fully resolved and located in the 2D separation space with excellent library matches, even though the underlying matrix was very complicated and would have strongly interfered in a 1D separation analysis. This will allow facile profiling of the reaction procedure for ecstasy synthesis.