Abstract: LC-MS/MS was applied to the determination of residual amounts of 11 mycotoxins in milk.The sample was extracted and protein precipitated with acetonitrile,and then fat was removed by n-hexane,dried with anhydrous sodium sulfate,cleaned up with M160 cartridges.Agilent Eclipse XDB-C18 chromatographic column was used as stationary phase,and the mixture of methanol and water mixed in different ratio was used as mobile phase in gradient elution.Multi-reactions monitor was adopted in MS/MS.Linear relationships between values of peak area and mass fraction of the 11 mycotoxins were kept in the same range within 4.0 μg·kg-1,with detection limits (3S/N)in the range of 0.001-0.006 ng.Values of recovery found by standard addition method were in the range of 60.1%-95.2%,and values of RSD′s (n=6) in the range of 3.2%-9.6%.