A new method was established for the determination of two kinds of guanidines vulcanization accelerators,1,3 diphenyl guanidine（DPG） and 1,3 di o tolylguanidine（DOTG） in synthetic rubber materials by high performance liquid chromatography（HPLC）.The samples were extracted by soxhlet extraction with methanol,and separated on a C18 column with acetonitrile-phosphate buffer as mobile phase by gradient elution.The UV detection wavelength was set at 235 nm,and the external standard method was used for quantitative analysis.There were good linear relationships for the two componds in the concentration range of 2-50 mg/L with their correlation coefficients both 0999 9.The limits of detection of the method（MLODs） were 30 mg/kg and 40 mg/kg,respectively.The average recoveries for the analytes were in the range of 824%-945%,with the relative standard deviations（RSD,n=5） of 10%-33%.This method was simple,rapid and reliable,and was suitable for the determination of DPG and DOTG residues in synthetic rubber materials．