The polar non-volatiles in the oxidized chicken fat prepared by control oxidation technology were analyzed by solid phase extraction (SPE) combining with liquid chromatography and atmosphere pressure chemical ionization mass spectrometry (LC-APCI-MS) as well as liquid chromatography and electric spray ionization mass spectrometry (LC-ESI-MS). Total of thirty-five kinds of oxidized compounds from glycerides classified as four types including bi-hydroperoxides, mono-hydroperoxides, diacylglycerols and epoxides were identified, among which mono-hydroperoxides (23 kinds) dominated. The mono-hydroperoxides in the oxidized chicken fat were quantified using mono-hydroperoxide of trilinolein as the external standard by LC-APCI-MS. The mono-hydroperoxides in the oxidized chicken fat turned out to be 121.36 mg/kg in total, whereby the mono-hydroperoxides of linoleoyl-dioleoyl-glycerol ranked the highest (45.05 mg/kg). The results indicated that the control oxidation technology was a kind of mild oxidation process, since the oxidized chicken fat was mainly the important flavor precursors of mono-hydroperoxides of triglyceride.