A high performance liquid chromatography with tunable ultraviolet method（HPLC-UV） was developed for the quantification of thiocyanate in milk products and raw materials.Samples were purified and extracted by Oasis WAX SPEs followed by protein precipitation with acetic acid.The purified solution was separated on a symmetry C18 column using methanol-phosphatic solution（containing ion pair reagent） as mobile phase,and analyzed by the internal standard method at a detection wavelength of 231 nm.Under the optimal conditions,the linear range for thiocyanate was in the range of 0.2-50 mg/L with correlation coefficient more than 0.999.The limit of detection for thiocyanate was 0.05 mg/kg,and the limit of quantitation（LOQ） was 0.15 mg/kg.The recoveries at spiked concentration levels of 1,5,25 mg/kg were in the range of 77%-104%.With the advantages of excellent reproducibility,high sensitivity and good practicability,this method could be used as a routine detection in practice.