Mass spectrometry is a chemical analytical method of determining organic substances by comparing their mass spectrum with mass spectra found in system libraries. In the case of biological products, substances of interest, like organophosphorus compounds, must be separated and identified for rapid and good medical measures (antidotism procedures) in acute intoxication case. A gas chromatograph coupled with a Varian mass spectrometer (GC-MS), was used to develop the application. The proposed objective is presenting the medical applicability in acute organophosphorus compounds intoxication management of the GC/MS method (gas chromatography coupled with mass spectrometry) as a separation and identification method for these compounds and their metabolites in urine samples.