A double internal standard quantitative method of capillary GC-MS was established for the determination of nicotine using campor and m cresol as the double internal substances.The result indicated that，under the same chromatographic conditions，the linear correlation coefficient of nicotine obtained from the double internal standard quantification curves was better than that obtained by the single internal standard method.This may be due to one more volatile substance as internal standard resulting in the rapid uniform distribution of samples partial pressure in the injection chamber.The effects of reducing the concentration of one standard and the location of the analyte peaks appeared on the correlation of the quantitative linear curve were also discussed.Therefore，it could be concluded that the double internal standard method coupled with quantitative capillary analysis can effectively eliminate the discrimination effect as injectting sample，and improve the accuracy of quantitative analysis.