Abstract: In order to accurately determine 1,2-propylene glycol,glycerol and triethylene glycol in cigarette filler,a dispersive solid-phase extraction-gas chromatography-mass spectrometry(d-SPE-GC/MS) method was developed.The humectants in cigarette filler were extracted by mechanically shaking with methanol,and the extraction was cleaned up by primary-secondary amine(PSA) and MgSO4 based d-SPE before GC/MS analysis and subsequently quantified with an internal standard method.The results showed that:The three humectants possessed good linear correlation(R² more than 0.999) within 0.0200-3.240 mg/mL,the average spiked recoveries ranged from 97.4% to 113.1% with the relative standard deviation lower than 7% and the limits of detection(LOD) from 2.27 to 22.80 μg/g.The coefficients of variation of intra-laboratory repeatability ranged from 2.3% to 6.7% and that of inter-laboratory reproducibility from 4.7% to 16.5%,through Cochran's Test and Grubbs' Test of experimental data from 4 laboratories and 6 test samples.This method is suitable for the simultaneous determination of 1,2-propylene glycol,glycerol and triethylene glycol in cigarette filler.