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Objective: The metabolism of drugs leads to more polar compounds, facilitating urinary elimination. Few drugs are recovered unchanged in the urine. Often, to highlight a chemical submission, the toxicologist receives blood and urine for events dating back to several days to a week. If the time between the events and the biological sample is long, the chance of highlighting a product is small. The aim of this study was to establish a protocol to obtain spectral information on metabolites of psychoactive drugs excreted in large quantities in the urine. Methods: The urines of patients who ingested a massive amount of a drug are analyzed by liquid chromatography-hybrid quadrupole timeof- flight mass spectrometry (UPLC QTOF XEVO G2). The MSe mode performs a double simultaneous acquisition: a low-energy acceleration to obtain the exact mass of compounds, the second at high acceleration energy to fragment all of the compounds. The data are processed by specialized software for research and characterization of metabolites (MetaboLynxTM), and analysis of collision fragments (MassFragment). Results: In the urine of a patient who ingested a massive amount of bromazepam, it was possible to characterize three major metabolites. Also, after a massive ingestion of alimemazine it was possible to characterize five major metabolites. Conclusion: Enlargement of the detection window of a compound in urine is possible by the characterization of its metabolites excreted in large amounts. [ABSTRACT FROM AUTHOR]