A systematic procedure for the determination of methaqualone and its metabolites in blood and urine by UV spectrophotometry, GC and GC/MS was developed. Urine and blood samples were from a suicidal patient who ingested 18 tablets of methaqualone. Both solid phase and liquid-liquid extractions were used in the extraction and clean-up of the samples. The total amount of methaqualone and its metabolites was measured by UV spectrophotometry. The amount of parent methaqualone was quantitated by GC/FID. Methaqualone and its 10 metabolites including two acetyl metabolites were found in urine and blood. This procedure is useful for monitoring drugs in emergency treatment.