Abstract: A method of GC for the determination of residual aldicarb in smoke of cigarettes was proposed.The total particulate matters (TPM) and gas phase matters in mainstream smoke of cigarettes were trapped by smoking machine,and the aldicarb collected was extracted with methanol.Aldicarb in the extract obtained was oxidized by H2O2,purified by extraction with CH2Cl2 to avoid interference,separated on DB-1701 capillary column and determined with PFPD detection.The quantitative analysis was carried out by external standard method.The detection limit (3S/N) of the method found was 0.01 μg·g-1.The values of recovery and RSD′s (n=6) of aldicarb were found in the range of 99.0%-101.0% and 4.7%-10.2% (in TPM);97.7%-99.3% and 5.4% to 9.6% (in gas phase),respectively.