A method for determination of organic solution residue in docetaxel using headspace capillary gas chromatog. was established.The conditions were: DB-624 capillary column (30 m × 0.32 mm × 1.8 μm), vaporization room temperature was 200°, determination room temperature was 250°, flow rate was 1.2 mL/min-1, and sample size was 0.16 mL.The determination limit of methanol, ethanol, acetone, dichloromethane, n-hexane, Et acetate, THF, and pyridine was 1.2, 6, 2, 4.8, 116, 1.2, 288, and 2 mg/L, and the recovery was 91.10%, 102.48%, 100.71%, 102.17%, 103.34%, 99.86%, 99.49%, and 100.39%, resp.