OBJECTIVE To establish a method for detection of plasma total homocysteine with HPLC. METHODS The chromatography analysis was carried out using a Symmetry Shield RP18. The mobile phase was sodium acetate (0.08 mol/L) and methanol (1%) and we utilized a HPLC system with fluorescence detection of plasma homocysteine derivatized from reaction with 7-fluorobenzo-2-oxa-1,3-diazole-4-sulphonate (SBD-F). RESULTS The average recoveries were 95.8 - 100.8% and the relative standard deviations were 1.2-2.0%. CONCLUSIONS The results showed it to be a rapid and accurate method for the determination of homocysteine level in plasma.