Abstract: The HPLC-MS fingerprint of raw milk extracted by acetonitrile was established to evaluate the quality of raw milk．A total of 11 peaks had been identified. The methodology was studied by the relative peak area and relative retention time with No. 7 peak as the reference. The results showed that the fingerprint established by this method has reasonable precision, reproducibility and stability with the relative standard deviations (RSDs) less than 0.79% for the relative retention time and less than 2.84% for the relative peak area．This method has provided a feasible analytical approach to explore the overall quality characteristics of raw milk.