Organophosphorus pesticides (OPs), are beingwidely used in agriculture, can cause toxic effects to humans and animals. The indiscriminate use of pesticides has generated numerous environmental problems. Especially, in the long term, it can cause serious harm in ecosystems and their associated individuals. The purpose of this investigation was to determine if the milk that is commercialized in the city of Cartagena de Indias has residual concentrations of organophosphorus pesticides. Seven milk samples were analyzed, e.g. six types of pasteurized milk of different brands and one type of raw milk obtained from a herd of the municipality of Maria la Baja, Bolivar, Colombia. The extraction technique used was solid phase microextraction (SPME) in headspace (HS) mode and the methods employed for separation and identification of the compounds were gas chromatography (GC) with flame ionization detector (FID) and mass spectrometry detector (MSD). This method proved advantageous in its application because of its environmentally soundness and facility in application and its confirmed accurate results. Organophosphorus compounds were not detected in the milk samples.