A selective and sensitive technique has been developed for detecting and identifying 11-nor-delta-9-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in human urine. Using a new, "mixed-mode", bonded silica gel, solid-phase extraction column cartridge, THC-COOH was selectively isolated from urine components. Following extraction, the presence of THC-COOH was confirmed and quantitated using gas chromatography-mass spectrometry (GC-MS) or gas chromatography-flame ionization detection. A linear quantitative response curve for THC-COOH was generated over a concentration range of 10 to 300 ng/ml. Overall extraction efficiency averaged greater than 85% and the quantitative response curve exhibited a correlation coefficient of 0.999. The limit of detection and identification using GC-MS for the drug metabolite was found to be six times below the present NIDA guidelines cut-off concentration of 15 ng/ml.