Abstract: A method for the separation and identification of 13 beta- blockers using GC/MS and GC/NPD are described. The TFA and TMS derivatives were prepared by adding TFAA, MSTFA and MBTFA to the standard drugs. The mixture was heated at 65℃ for 20 min and chromatographed on FS capillary columns (HP-5).Preliminary results show that the derivatization with MSTFA is better than that with TFAA or MBTFA. There is not much difference between TFAA and M BTFA derivatization. The method is reliable, rapid and simple and may be used to screen these drugs and further applied to the analysis of biological fluids such as plasma and urine.