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A procedure for alminoprofen, loxoprofen, tiaprofenic acid (propionic acid derivatives) and their metabolites in urine has been developed using a high-performance liquid chromatography / mass spectrometry (LC/MS) with sonicspray ionization (SSI, negative mode). These drugs and their metabolites showed satisfactory results of separation and sensitivity by LC/MS using Mightysil RP-18 column with 10mM acetic acid: methanol (35:65,v/v) as a mobile phase at 0.08 ml/min at 35degreesC. The extraction procedure of these drugs and metabolites added in the human urine was performed with Oasis(R) MAX cartridge. Yields of column extraction of 500 mul of human urine samples (containing 5 mug of drugs) were 58.3-105.2%. The detection limits were 0.7-2.9 mug/ml.