Abstract: Procedures for the separation and identification of 12 narcotic analgesics and 2 CNS-stimulants are described using GC/FID, GC/NPD and GC/MSD.The TFA and TMS derivatives were prepared by adding TFAA,MB TFA and MSTFA to the standard drugs.The mixture was heated at 70℃ for 30 min and chromatographed on FS capillary columns(SE-54,HP-5). Preliminary results show that all the derivatization with TFAA is better than that with MBTFA, but not much different from MSTFA derivatization. The method is reliable, fast and simple and may be used to screen these drugs and further applied to the analysis of biological fluids such as plasma and urine.