Abstract: In order to assess the exposure to acrylamide of a smoker during smoking accurately, an SPE-HPLC-MS/MS method was developed for determining the mercapturic acid (MA) metabolites, N-acetyl-S-(2-carbamoylethyl)-L-cysteine (AAMA) and N-acetyl-S-(2-carbamoyl- 2-hychoxyethyl)-L-cysteine(GAMA), of acrylamide in human urine.The contents of AAMA and GAMA in the urine of smokers and nonsmokers were determined, and the correlation analysis between the determined data and the acrylamide exposure evaluated by filter analysis was conducted. The results showed that: 1)The method was accurate and sensitive with the intra-day and inter-day precisions less than 7% and 11%, respectively. The recoveries ranged from 94.9% to 100.0%, and the detection limits of AAMA and GAMA were 0.6 and 0.1 ng/mL, respectively. 2) The mean value of AAMA and GAMA in smokers 'urine was three times the value in nonsmokers'. 3) The content of AAMA, the main metabolite of acrylamide, in urine had a certain correlation(R=0.567, P < 0.03) with the acrylamide exposure determined by filter analysis.