A new cryogenic instrument was designed for the trapping of aerosols such as cigarette mainstream smoke at low temperature. The technique enabled the trapping of the mainstream smoke of a single cigarette and the particulate and vapor phases were trapped simultaneously. 2R4F reference cigarettes were smoked under International Standard Organization (ISO) regime and trapped at low temperature using the cryogenic instrument. After trapping, the mainstream smoke of the 2R4F reference cigarette was diluted with a solvent and selected smoke components could be quantified using gas-mass spectrometry (GCMS) and high-performance liquid chromatography (HPLC). The capability of the instrument for trapping the mainstream smoke was demonstrated. The feasibility of the procedure for the detection and the quantification of a large range of smoke components including carbonyls, alkaloids and organic volatile compounds (VOC) in the mainstream of a single cigarette was also shown.