Abstract: OBJECTIVE To establish a method for determination of residual organic solvents from the AB-8 macroporous adsorption resin in Jiweiling freeze-dry powder, including n-hexane, benzene, toluene, 1,2-xylene, 1,3-xylene, 1,4-xylene, stryene, divinylbenzene. METHODS The residual organic solvents were analyzed by headspace gas chromatography on AT-WAX capillary column, FID detector and by temperature programming. RESULTS The eight residual organic solvents were completely separated. There was good linearity in resparatively linear ranges and r was 0.999 1-0.999 8, the RSD of precision was less than 3%, the samples were stable in 8 h, the detection limits were n-hexane 0.08 μg·mL^-1, benzene 0.025 μg·mL^-1, toluene 0.04 μg·mL^-1, (1,2-; 1,3-; 1,4-)xylene 0.2 μg·mL^-1, stryene 0.4 μg·mL^-1, divinylbenzene 0.1 μg·mL^-1. CONCLUSION The method is simple and accurate and can be used to detect and control the organic residul solvents from the AB-8 macroporous adsorption resin in Jiweiling freeze-dry powder.