Abstract: Three kinds of chemically bonded micro-porous silica (10 um partisil ODS-2, 10 μm GYT-C18 and 5 μm GYT-C₁₈) were used for separation of amino acids and amines diastereoisomers, 5μm and 10 μm GYT-C₁₈, prepared in our Institute, with good efficiency. The theoretical plates of Partisil ODS, 10μm and 5μm GYT-C₁₈ are 10000plates/m, 46000plates/m and 53000plates/m, respectively. Five racemic amino acids were separated as the diastereoisomeric mixture of D-camphor-β-suphonyl-p-nitrobenzyl ester and two racemic aralkylamines as N-D-camphor-β-sulphonylamines. The column slurry-packed with 10 μm GYT-C₁₈ gave the most favorable results. For seven racemates tested, six pairs of diastereoisomers gave baseline separation.The experimental data showed that no conclusive correlation between elution order and absolute configurations could be determined.