A method for determination of raceanisodamine,scopolamine and()-hyoscyamine by LLE-GC-MS was established.MethodsDatura was filtered after ultrasonic extraction with 2 mol/L hydrochloric acid for 30 min. The filtrate was extracted three times with chloroform after adjusting pH to 9 with concentrated aqueous ammonia. The extract was evaporated to dryness and diluted to constant volume before determination. ResultsThere was a good linearity between the peak area and the concentration of raceanisodamine, scopolamine and()-hyoscyamine within the range of 0.1-0.5 mg/ml, the correlation coefficients were 0.998 1-0.999 5, the recoveries of spiked samples at 0.2 mg/ml and 0.4 mg/ml to flowers and leaves of datura were ranged from 76.7% to 119.0%, RSDs were ranged from 0.8% to 7.3%, and the detection limits were ranged from 0.1 to 1.0 μg/kg. ConclusionThe method was simple, rapid and reliable. It could be applied to determine raceanisodamine, scopolamine and()-hyoscyamine in datura.