Widespread occurrence of pharmaceuticals has started to attract attention as aquatic micropollutants that might have been affecting the ecological system in trace amounts. The risks associated with their introduction into wildlife habitats is becoming an important issue for both regulators and the pharmaceutical industry, because of incomplete elimination of pharmaceuticals wastewater and their metabolites. In this work monitoring of some pharmaceutical residues in industrial wastewater such as (caffeine, paracetamol, dexamethasone and naproxen) was carried out. The identification and quantification of chemical and pharmaceutical residues was investigated using GC/MS spectrometer and liquid chromatography-based tandem mass spectrometry LC/MS/MS spectrometer with electrospray ionization (ESI) .The study recorded the presence of different types of pharmaceutical residues with different concentration levels in wastewater .The concentration level of dexamethasone in wastewater were detected at 254 ng/ml, for paracetamol at 7325 ng/ml , for caffeine at 9356 ng/ml and for naproxen at 2 ng/ml . These concentrations representing about 500 fold higher than international safety margin of treated wastewater.