The use of biomass and other solid material as a source of energy is associated with some deleterious effects consequent to incomplete combustion associated with poor ventilation leading to production of a number of chemical compounds that are known or suspected to be a health threat. This study reports the screening of the formation of the polycyclic hydrocarbons during pyrolysis of the fuel materials, namely, coal, dung and wood, commonly used as fuel in rural areas in Lesotho, under poor aeration using a simple in-house pyrolysis unit The method demonstrated sufficient linearity for the standards with correlation coefficient, R2 ≥ 0.9884 and repeatability (%RSD ≤ 15 %) of the real samples used, coal demonstrated production of naphthalene and pyrene, while from the cake dung formation of naphthalene was detected. Despite not being extensive, the results form a basis for a more rigorous study including employing more identification tools, such as mass spectrometry that enables identification and a better detection of low levels of the analytes.