OBJECTIVE To determine the residual organic volatile solvents in rifampin and lornoxicam.METHOD S The samples were injected on sillica capillary column by headspace sampler with FID detector.The determination of rifampin was performed on a HP5 5% phenyl methyl siloxane.The column temperature was 50℃.The determination of lornoxicam was performed on a AC 20 polyethylene glycol column which was kept the initial temperature at 50℃,then raised to 165℃ at the rate of 10℃·min^-1 and sustained for 5 min.RESULTS The correlation r in methanol,acetone,chloroform and butanol was respectively 0.999 9,0.999 9,0.998 4 and 0.999 8.The recovery was 96.0%,97.3%,81.1% and 93.9% with RSD 2.7%,1.9%,8.8% and 2.5%,(n=5) respectively.CONCLUSION The method appeared to be sensitive and accurate,and can be used for the determination of the residual organic volatile solvents in rifampin and lornoxicam.