Descriptions of the materials and methods used in the procedure address synthetic procedures, instrumentation, the extraction procedure, and standard curve generation. A solid phase extraction (SPE) method was used to extract cocaine, AEEE, and related metabolites from the deceased's urine. SPE on a 1 ml urine sample from the decedent, followed by gas chromatography-mass spectrometry (GC-MS) detected AEEE. Other metabolites identified by GC-MS included cocaine, cocaethylene, and anhydroecgonine methyl ester (AEME). To determine whether some or all of the AEEE was artifactually produced in the heated GC injector port, an alternative liquid chromatography-mass spectrometry (LC-MS) method was developed. LC/MS following SPE found at least 50 ng/ml of AEEE in the extract. The mass fragmentation of AEEE detected in the urine was compared to spectra of authentic, synthesized compound. AEEE is thus a potential additional forensic marker for the co-abuse of smoked cocaine and ethanol. LC-MS provides the basis for a useful analytical method in forensic cases involving suspected free-base cocaine/ethanol use. 36 references