Abstract: A rapid method for the determination of related components in mainstream cigarette smoke, including carbon monoxide, 4-(methylnitrosamine)-3-pyridine-1-butanone (NNK), phenol, crotonaldehyde, ammonia and hydrogen cyanide, was set up. Solvent trapping and filter trapping methods were used to trap on the smoking machine at the same time. Ammonia, hydrogen cyanide and crotonaldehyde were trapped by the solvent trapping method, and NNK, ammonia, hydrogen cyanide and phenol were trapped by the filter trapping method. Then the samples were detected using high-performance liquid chromatography (HPLC), ion chromatography (IC) and liquid chromatography/mass spectrometry (LC/MS). Carbon monoxide was detected on the non scattering infrared detector of the smoking machine. The test results showed that comparing with the tobacco industry standard method for the detection of 6 related components in cigarette smoke, the relative standard deviation (RSD) of NNK was less than 6.0%, and RSD of other detection results were less than 3.0%, which is suitable for the determination of the content of related components in mainstream cigarette smoke.