Abstract:A high performance liquid chromatographic -HPLC- method was developed for determining thiocyanate in milk. HPLC analysis was performed on a Dionex IonPac AS19 -4mm×250mm- anionic chromatography column with DAD detector, 005mol/L Na2HPO4 solution was used as mobile phase -pH 93- at a flow rate of 08mL/min, sample loading amount was 10μL, and detection wavelength was 218nm. The method exhibited a limit of detection of 05μg/mL and a linear range of 5-100μg/mL. Spike recoveries of thiocyanate in milk powder and liquid milk at two levels ranged from 671%-1018%, with RSDs -n=3- less than 44%.