Polycyclic aromatic compounds (PACs) are a structurally diverse class of environmental contaminants many of which are persistent (P), bioaccumulative (B) and inherently toxic (T). They can be formed from natural activities (such as volcanic activities and wildfires) or human activities (incomplete combustion and power plants). Due to their PB&T properties, PACs are considered an ecological threat, and there is great interest in measuring PACs in environmental compartments especially in biological samples. Because of their ability to accumulate contaminants, birds are an invaluable bioindicator of environmental health, and many countries use them in their environmental monitoring programs. The focus of my research was to develop and validate new approaches to the analysis of PACs in bird matrices and to evaluate if bird feathers can be used as a non-invasive matrix for the determination of PACs. Extraction of PACs from serum and blood, was achieved using microbead beating homogenization, and for feathers, I used pressurized fluid extraction. Detection and quantitation of PACs were based gas chromatography-tandem mass spectrometry. The performance characteristics of my methods were done in strict accordance with the EURACHEM guide - The Fitness for the purpose of Analytical Methods. The importance of my research is the development of more accurate, less time-consuming and more cost-effective approaches to the analysis of PACs in these matrices. Finally, my research is a reasonable first step toward the use of feathers as a non-invasive approach for monitoring the concentration of PACs in the environment.