Comprehensive two-dimensional (2D) gas chromatography (GCxGC) analysis is an innovative technology developed at RMIT University which can separate and detect very low levels of complex, volatile substances such as drugs of abuse. The aim of this project is to determine whether GCxGC analysis is suitable for routine use in a forensic laboratory for profiling illicit substances. This report includes: evaluation of world anti-doping agency criteria for anabolic agent analysis by using comprehensive two-dimensional gas chromatography/mass spectrometry; organic impurity profiling of ecstasy tablets using GCxGC; the application of GCxGC in heroin and cocaine profiling. The results presented in this final report indicate that there is considerable scope to be optimistic about the future for profiling of illicit drug samples by using GCxGC technology.