Abstract: In the present study, amylose-tris(phenylcarbamate)(ATPC) and amylose-tris(3,5-dimethylphenylcarbamate)(ADMPC) were synthesized, and used as the chiral stationary phases upon adsorption over silica gel. These stationary phases offered a practically useful chiral column with a high enantiomer-separability. Amylose was allowed to react with an excess of phenylisocyanate or 3,5-dimethylphenylisocyanate in pyridine for 48 h. The carbamates obtained were dissolved and adsorbed on silica gel which had been treated with 3-aminopropyltriethoxysilane. The weight ratio of the carbamate to the silica gel was 0.45/2.55. The eight thio-glycidyl ethers were resolved on the two chiral stationary phases. Separation was carried out with a hexane/2-propanol mixture at a flow rate of 1.0 mL/min at room temperature. The effects of chiral stationary phases and 2-propanol concentration on the retention and resolution were investigated.

Key words: HPLC, Amylose-chiral stationary phase, Racemic thio-glycidyl ether, Enantiomeric separation