Gas chromatographic method was investigated for the chiral separation of several $eta$-blockeros(atenolol, betaxolol, bisoprolol, metoprolol and pindolol) using (-)-$alpa$-methoxy-$alpa$-(trifluoromethyl)phenylacetyl chloride as a chiral derivatizing agent for amino group. Prior to N-acylation, hydroxyl group was converted into O-silyl ethers by react with N-methyl-H-(taimethylsilyl)trifluoroacetamide. The reaction was selective and rapid and the diasteromeric derivatives were well separated by capillary gas chromatography. (R)-isomers were eluted faster than (S)-isomers when (-)-$alpa$-methoxy-$alpa$-(trifluoromethyl)phenylacetyl chloride was used as the chiral derivatizing agent. But in the opposite sequence when (+)-$alpa$-methoxy-$alpa$-(trifluoromethyl)phenylacetyl chloride was used. No racemization was found during the reaction.