A　new　method　for　separation　and　determination　of　amygdalin　and　its　epimer　(neoamygdalin)　in　the　epimerization　of　amygdalin　by　MEEKC　is　proposed.　For　the　chiral　separation　of　amygdalin　and　neoamygdalin,　a　running　buffer　composed　of　80　mM　sodium　cholate,　5.0%　v/v　butan-1-ol,　0.5%　v/v　heptane　and　94.5%　v/v　30　mM　Na2B4O7　buffer　(pH　9.00)　is　proposed.　Under　optimum　conditions,　the　basic　separation　of　amygdalin　and　neoamygdalin　can　be　achieved　within　7　min.　The　calibration　curve　for　amygdalin　showed　excellent　linearity　in　the　concentration　range　of　20-1000　mu　g/mL　with　a　detection　limit　of　5.0　mu　g/mL　(S/N　=　3).　The　epimerization　rate　constant　of　amygdalin　in　basic　microemulsion　was　first　determined　by　monitoring　the　concentration　changes　of　amygdalin,　and　the　epimerization　rate　constant　of　amygdalin　was　found　to　be　2　x　10(-3)　min(-1)　at　25　degrees　C　under　the　above　optimum　microemulsion　conditions.