The analysis of smoke particulate matter is being performed on different kinds of cigarettes. Cigarette smoke is generated using an in-house custom made smoking machine. Samples are collected on silicate filter pads and run through a detailed extraction procedure before being analyzed by gas chromatography-mass spectrometry (GC-MS). The analytes of interest are nine suspected carcinogens and EPA priority pollutants: nicotine, fluorene, anthracene, pyrene, benzo[a]anthracene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, and perylene. The major developments in this research are the optimization of the GC-MS instrumentation and extraction procedure involving solid phase extraction (SPE)-based techniques. Deuterated molecules of the carcinogens are used as internal surrogate standards and calibration curves are established in order to quantify concentrations in the collected smoke samples. Additional focus is on the chromatographic resolution of benzo[b]fluoranthene and benzo[k]fluoranthene using the GC-MS. This work will help researchers understand the deposition of carcinogens in the lungs that are resultant of the smoking process.