On the basis of the optimization of solid phase extraction adsorbent, eluting solvent types and amounts, a gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) method was established for the determination of 213 pesticide residues in milk and milk power. The samples were extracted by acetonitrile, cleaned-up with an ENVI-Carb/NH2 solid-phase extractant, and determined by GC-MS/MS using external standard method. The linear ranges were from 10 to 1 000 μg/L for 197 pesticides, from 50 to 1 000 μg/L for the other 16 pesticides with the correlation coefficients higher than 0.99. The limits of detection (LODs, S/N = 3) varied over the range of 0.03 to 7.59 μg/kg, and limits of quantification (LOQs, S/N = 10) ranged from 0.10 to 21.94 μg/kg. The average recoveries in different matrices were in the range of 66.9% - 120.1% with the relative standard deviations (RSDs) of 1.23% - 17.6%. This method is simple, rapid, sensitive and reliable for meeting the requirements for the simultaneous identification and quantification of the multi-residues in milk and milk power.