In recent years there has been a growing interest in a much wider range of chemicals found in cigarette smoke, including constituents of both the vapour and particulate phases. This has been brought about by the requirement in British Colombia to publish the levels of 56 smoke constituents in both mainstream and sidestream cigarette smoke of all cigarette brands with over 2% of the total market. The list of chemicals comprises known carcinogens and irritants which it is claimed add to the risk of contracting a smoking related disease. Such interest has led to intense activity in smoking laboratories to develop procedures to trap and quantify these chemicals in smoke. Various procedures are described for the trapping; separation and extraction of mainstream cigarette smoke analytes using a semi-automated smoking machine (ASM 500). Methods for the analysis of smoke have been developed using such techniques as GC-MS, LC-MS, or LC with UV or fluorescence detection. Procedures for the determination of selected volatile compounds such as formaldehyde and hydrogen cyanide are also described. Typical yields of the compounds of interest for various cigarette designs will be discussed with specific reference to the yields of the CORESTA CM3 monitor cigarette.