Pharmaceuticals are chemical substances used in the treatment and prevention of diseases. They are considered as new pollutants because they do not have defined a regulatory legal dose for releasing treated wastewater into the environment. Due to increased pharmaceutical consumption they are present in the water, soil, sediment and in the environment. The reason is that small molecules of pharmaceuticals can not be completely removed by the classical wastewater treament methods of the pharmaceutical industry and they are retained in the active sludge of wastewater treatment. Therefore, it is necessary to introduce leagally prescribed maximum concentration of pharmaceuticals in the environment but it is also necessary to monitor the concentrations of the pharmaceuticals before and after wastewater treatment of the pharmaceutical industry. The concentration of pharmaceutcals in active sludge should be monitored and the sludge should be disposed in adequate procedure after the usage. For this purpose it is necessary to develop analytical methods for extraction of pharmaceuticals from real samples and quantitatively and qualitatively determine the pharmaceuticals by appropriate tehniques. The pharmaceuticals used in this paper are: antihelminitics (albendazole, febantel, praziquantel), antibiotics (azitromycine, eritromycine, cefdinir, chlaritromycine, nitrofurantoin), chemoterapeutic agent (hydroxychloroquine) and antiemetic (metoclopramide). The aim of this paper is to determine the optimum conditions for extraction of the pharmaceuticals by the method of agitation from the active sludge. Optimized parameters are type and volume of solvent, time of extraction, sample and solvent ratio and pH value. The quantitative and qualitative analysis of the pharmaceuticals was preformed by tandem chromatographic systems: high preformace liquid chromatography with diode array detectors (HPLC-DAD) and high preformance liquid chromatography with mass spectrometry (HPLC-MS/MS). The best results were achived with solvent systems: methanol:acetonitrile, methanol:acetone, methanol:water and methanol:hexane with 0,5 g of sample with a solvent volume of 3 mL. However, with this method the achieved efficiencies were up to 30 % which is not satisfactory. The method as such was neither validated nor recommended for routine use despite the simplicity and low cost of the extraction method.