A　method　was　developed　for　the　chiral　separation　of　dipeptides　with　two　chiral　centers.　Although　all　analyzed　peptides　contain　chromophores　and　they　can　be　detected　by　UV-adsorption　detection　without　any　derivatization,　the　chiral　separations　were　not　achieved　for　non-derivatized　peptides　using　the　same　chiral　selectors　and　experimental　conditions.　In　this　paper,　these　dipeptides　were　precolumn　derivatized　by　using　naphthalene-2,　3-dicarboxyaldehyde　as　a　tagging　reagent.　In　the　presence　of　2-hydroxypropyl-beta-CD　and　sodium　deoxycholate,　naphthalene-2,3-dicarboxyaldehyde-tagged　dipeptide　enantiomers　were　well　resolved　by　MEKC.　Good　separation　of　all　enantiomers　was　obtained　within　14　min.　The　proposed　method　was　applied　to　chiral　separation　of　dipeptide　enantiomers　in　spiked　human　serum　samples.