Pharmaceuticals are the chemical compounds most commonly used in the pharmaceutical industry and they are used to treat or prevent diseases of humans and animals. They are referred to as new pollutants because they have not been researched so far and there are no legal regulations on their release into the environment. They are chemical substances that are released to the environment in larger quantities and pose a potential danger to the living world. Although we are not familiar with the way they behave in the environment, it is very important to develop the best methods of qualitative and quantitative determination of active pharmaceutical substances in different environmental constituents as well as methods for their elimination. This paper studies the removal of the pharmaceuticals by ultrasonic extraction from the active sludge. The analyzed active sludge did not contain pharmaceutical. It was afterwards contaminated with the following pharmaceuticals: albendanzole, febantel, praziquantel, nitrofurantoin, cefdinir, hydroxychloroquine and metoclopramide. Ultrasonic extraction was performed by using different solvents: methanol, ethanol and methanol-water at a ratio of 1:1. Separation and qualitative analysis of the pharmaceuticals were conducted by high performance liquid chromatography (HPLC). The best results of ultrasonic extraction was obtained at a temperature of 30 °C for 60 min, and the most preferred solvent for extraction was methanol. However, none of the solvents yielded satisfactory results, and ultrasonic extraction, as a method of removing pharmaceuticals from active sludge, is not recommended. The method was validated by determining repeatability, renewability, boundary detection and boundary quantification.