OBJECTIVE　To determine the content of N,N-dimethyl-formamide,the residual organic volatile solvents,in micronazed gilibenclamide capsules.METHODS　Dissolved in dimethyl sulphoxide,2 μL sample solution was injected on a DB-1 (100% dimethyl-polysiloxane) sillica capillary column using nitrogen as the carrier gas.Keep the initial temperature at 150℃ for 14 min,then it was raised to 200℃ at the rate of 40 ℃*min-1,sustained for 12 min.The injection port and FID detector were 210℃ and 240℃.Under this condition,N,N-dimethyl formamide and the internal standard tetrahydrofuran were separated completeh.RESULTS　The linear range of N,N-dimethyl formamide was 35.19～28.15 μg*mL-1,and the LOD was 8.8 μg*mL-1.The precisions was 1.9%.The recovery of N,N-dimethyl formamide was 101.4%.Three batches of sample were analysed.CONCLUSION　After validation,the method was proved to be accurate,sensitive and reliable.It is quite suitable to be used in the analysis of the N,N-dimethyl formamide in micronazed gilibenclamide capsules.